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Sample records for twenty-four-hour urine samples

  1. Twenty-Four-Hour Urine Osmolality as a Physiological Index of Adequate Water Intake

    Directory of Open Access Journals (Sweden)

    Erica T. Perrier

    2015-01-01

    Full Text Available While associations exist between water, hydration, and disease risk, research quantifying the dose-response effect of water on health is limited. Thus, the water intake necessary to maintain optimal hydration from a physiological and health standpoint remains unclear. The aim of this analysis was to derive a 24 h urine osmolality (UOsm threshold that would provide an index of “optimal hydration,” sufficient to compensate water losses and also be biologically significant relative to the risk of disease. Ninety-five adults (31.5 ± 4.3 years, 23.2 ± 2.7 kg·m−2 collected 24 h urine, provided morning blood samples, and completed food and fluid intake diaries over 3 consecutive weekdays. A UOsm threshold was derived using 3 approaches, taking into account European dietary reference values for water; total fluid intake, and urine volumes associated with reduced risk for lithiasis and chronic kidney disease and plasma vasopressin concentration. The aggregate of these approaches suggest that a 24 h urine osmolality ≤500 mOsm·kg−1 may be a simple indicator of optimal hydration, representing a total daily fluid intake adequate to compensate for daily losses, ensure urinary output sufficient to reduce the risk of urolithiasis and renal function decline, and avoid elevated plasma vasopressin concentrations mediating the increased antidiuretic effort.

  2. Twenty-four-hour urine constituents in stone formers: A study from the northeast part of Peninsular Malaysia

    OpenAIRE

    N S Hussein; S M Sadiq; M D Kamaliah; A W NorAkmal; M N Gohar

    2013-01-01

    Urolithiasis is a common disease with increasing incidence and prevalence world-wide, probably more common in industrialized countries. The metabolic evaluation of 24-h urine collection has been considered as part of the management of urinary stone patients. The aim of this study was to evaluate the 24-h urine constituents in stone formers and its relation to demographic data in the northeast part of Peninsular Malaysia. One hundred and six patients were recruited in this study from two hospi...

  3. Twenty-four-hour urine constituents in stone formers: A study from the northeast part of Peninsular Malaysia

    Directory of Open Access Journals (Sweden)

    N S Hussein

    2013-01-01

    Full Text Available Urolithiasis is a common disease with increasing incidence and prevalence world-wide, probably more common in industrialized countries. The metabolic evaluation of 24-h urine collection has been considered as part of the management of urinary stone patients. The aim of this study was to evaluate the 24-h urine constituents in stone formers and its relation to demographic data in the northeast part of Peninsular Malaysia. One hundred and six patients were recruited in this study from two hospitals in the same geographical region; 96 patients fulfilled the inclusion criteria and an informed consent was obtained from all subjects. The 24-h urine was collected in sterile bottles with a preservative agent and calcium, oxalate, citrate, uric acid, magnesium and phosphate were tested using commercial kits on a Roche Hitachi 912 chemistry analyzer. The age (mean ± SD of 96 patients was 56.45 ± 13.43 years and 82.3% of the patients were male while 17.7% were female. The 24-h urine abnormalities were hypercalciuria (14.5%, hyperoxaluria (61.4%, hypocitraturia (57.2%, hyperuricouria (19.7%, hypomagnesuria (59.3% and hyperphosphaturia (12.5%. Hyperoxaluria (61.4% was the most common abnormality detected during the analysis of 24-h urine constituents in contradiction to industrial countries, where hypercalciuria was the most common finding. The high frequencies of hypomagnesuria and hypocitraturia reflect the important role of magnesium and citrate in stone formation and their prophylactic role in the treatment of urinary stone disease in the given population.

  4. Twenty-four-hour urine constituents in stone formers: a study from the northeast part of Peninsular Malaysia.

    Science.gov (United States)

    Hussein, N S; Sadiq, S M; Kamaliah, M D; Norakmal, A W; Gohar, M N

    2013-05-01

    Urolithiasis is a common disease with increasing incidence and prevalence world-wide, probably more common in industrialized countries. The metabolic evaluation of 24-h urine collection has been considered as part of the management of urinary stone patients. The aim of this study was to evaluate the 24-h urine constituents in stone formers and its relation to demographic data in the northeast part of Peninsular Malaysia. One hundred and six patients were recruited in this study from two hospitals in the same geographical region; 96 patients fulfilled the inclusion criteria and an informed consent was obtained from all subjects. The 24-h urine was collected in sterile bottles with a preservative agent and calcium, oxalate, citrate, uric acid, magnesium and phosphate were tested using commercial kits on a Roche Hitachi 912 chemistry analyzer. The age (mean ± SD) of 96 patients was 56.45 ± 13.43 years and 82.3% of the patients were male while 17.7% were female. The 24-h urine abnormalities were hypercalciuria (14.5%), hyperoxaluria (61.4%), hypocitraturia (57.2%), hyperuricouria (19.7%), hypomagnesuria (59.3%) and hyperphosphaturia (12.5%). Hyperoxaluria (61.4%) was the most common abnormality detected during the analysis of 24-h urine constituents in contradiction to industrial countries, where hypercalciuria was the most common finding. The high frequencies of hypomagnesuria and hypocitraturia reflect the important role of magnesium and citrate in stone formation and their prophylactic role in the treatment of urinary stone disease in the given population.

  5. Twenty-four-hour blood pressure among Greenlanders and Danes: relationship to diet and lifestyle

    DEFF Research Database (Denmark)

    Jørgensen, Marit Eika; Pedersen, M.B.; Siggaard, Cecilie

    2002-01-01

    the influence of Arctic food and lifestyle on blood pressure. Four groups of healthy subjects were recruited for the study. Group I: Danes in Denmark consuming European food; group II: Greenlanders in Denmark consuming European food; group III: Greenlanders in Greenland consuming mainly European food; and group......, outdoor temperature, and lifestyle factors. Greenlanders have a lower 24-h diastolic blood pressure than Danes, and it is suggested that genetic factors are mainly responsible for the lower blood pressure level among Greenlanders. Twenty-four-hour blood pressure among Greenlanders and Danes: Relationship...... to diet and lifestyle - ResearchGate. Available from: http://www.researchgate.net/publication/11001663_Twenty-four-hour_blood_pressure_among_Greenlanders_and_Danes_Relationship_to_diet_and_lifestyle [accessed Oct 7, 2015]....

  6. Twenty-four hour Holter monitoring in finishing cattle housed outdoors.

    Science.gov (United States)

    Frese, D A; Thomason, J D; Reinhardt, C; Bartle, S; Rethorst, D; Loneragan, G H; Thomson, D

    2017-04-01

    Atrial premature complexes have been reported to be the most common arrhythmia in cattle and is suspected to be secondary to systemic disease, especially gastrointestinal disease. In order to properly identify pathologic arrhythmia in cattle, the normal rhythm and arrhythmia prevalence should be defined. The objective of this study was to determine the normal heart rate, rhythm, number of ventricular premature complexes (VPCs), and atrial premature complexes (APCs) in unrestrained Angus steers. Twenty-seven client owned steers with unremarkable physical examinations and serum biochemical analyses were used. Twenty-four hour Holter monitors, attached by a custom-made harness, were retrospectively evaluated. Three lead electrocardiographic registrations of good quality and normal sinus rhythm were obtained from all steers in the study. The mean heart rate was 66.8 bpm ± 16.4 bpm. Ventricular premature complexes were rare (noted in 14.8% of steers), and APCs were common (noted in 85% of the steers). Simple second degree AV block was observed in 18.5% of the steers. In summary, healthy steers have rare single VPCs, although it is possible for an individual animal to have apparent more frequent VPCs. Mean heart rate varies with a diurnal pattern similar to other species. Atrial premature complexes are the most prevalent abnormality observed in feedlot steers. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Twenty-four-hour esophageal pH monitoring in children and adolescents with chronic and/or recurrent rhinosinusitis

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    V.R.S.G. Monteiro

    2005-02-01

    Full Text Available Gastroesophageal reflux (GER disorder was studied in children and adolescents with chronic and/or recurrent rhinosinusitis not associated with bronchial asthma. Ten children with a clinical and radiological diagnosis of chronic and/or recurrent rhinosinusitis, consecutively attended at the Pediatric Otolaryngology Outpatient Clinic, Federal University of São Paulo, were evaluated. Prolonged esophageal pH monitoring was used to investigate GER disorder. The mean age of the ten patients evaluated (eight males was 7.4 ± 2.4 years. Two patients presented vomiting as a clinical manifestation and one patient presented retrosternal pain with a burning sensation. Twenty-four-hour esophageal pH monitoring was performed using the Sandhill apparatus. An antimony probe electrode was placed in the lower third of the esophagus, confirmed by fluoroscopy and later by a chest X-ray. The parameters analyzed by esophageal pH monitoring included: total percent time of the presence of acid esophageal pH, i.e., pH below 4 (<4.2%; total number of acid episodes (<50 episodes; number of reflux episodes longer than 5 min (3 or less, and duration of the longest reflux episode (<9.2 min. One patient (1/10, 10% presented a 24-h esophageal pH profile compatible with GER disorder. This data suggest that an association between chronic rhinosinusitis not associated with bronchial asthma and GER disorder may exist in children and adolescents, especially in those with compatible GER disorder symptoms. In these cases, 24-h esophageal pH monitoring should be performed before indicating surgery, since the present data suggest that 10% of chronic rhinosinusitis surgeries can be eliminated.

  8. Clean catch urine sample

    Science.gov (United States)

    ... opening of the vagina. To collect the urine sample: Keeping your labia spread open, urinate a small amount into the toilet bowl, then stop the flow of urine. Hold the urine cup a few inches (or a ...

  9. Twenty-four-hour profiles of metabolic and stress hormones in sheep selected for a calm or nervous temperament.

    Science.gov (United States)

    Rietema, S E; Blackberry, M A; Maloney, S K; Martin, G B; Hawken, P A R; Blache, D

    2015-10-01

    Even in the absence of stressors, temperament is associated with changes in the concentration of stress-responsive hormones and, possibly because of such changes, temperament can affect metabolism. We tested whether, in sheep bred for temperament for 14 generations, "nervous" females have greater concentrations of stress-responsive hormones in the absence of stressors than "calm" females, and whether these differences are associated with changes in the concentrations of metabolic hormones. In resting "calm" (n = 8) and "nervous" (n = 8) sheep, concentrations of cortisol, prolactin, leptin, and insulin were measured in blood plasma sampled via jugular catheter every 20 min for 24 h. The animals were individually penned, habituated to their housing and human handling over 7 wk, and fed before sampling began. Diurnal variation was evident for all hormones, but a 24-h cortisol pattern was detected in only 7 individuals. There was no effect of temperament on any aspect of concentrations of cortisol or prolactin, but "calm" animals had greater concentrations of insulin in the early afternoon than "nervous" animals (14.5 ± 1.1 vs 10.0 ± 1.6 μU/mL; P = 0.038), and a similar tendency was seen for leptin (P = 0.092). We conclude that selection for temperament affects the concentration of metabolic hormones in the absence of stressors, but this effect is independent of stress-responsive hormones.

  10. [Changes of twenty-four-hour profile blood pressure and its correction of patients with arterial hypertension on the background of combined antihypertensive therapy application].

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    Solomennchuk, T M; Slaba, N A; Prots'ko, V V; Bedzaĭ, A O

    2014-01-01

    The aim of this research was the study of efficiency and endurance antihypertensive therapy on the basis of fixed combination of enalapril and hydrochlorothiazide (HCTZ) and enalapril and HCTZ in combination with amlodipine according to the twenty-four-hour (? day-and-night) monitoring of blood pressure (? 24H BPM) of patients with arterial hypertension (AH) 2-3 severity. The study included 33 patients with 2-3 grade of hypertension (average age--54,40 ± 3.45 years). All patients performed ? 24H BPM before treatment and after 12 weeks of therapy. The combination of enalapril and HCTZ allowed to achieve target levels of blood pressure in 79% of patients, amlodipine additional purpose--in 86% of patients. We found that this therapy has a corrective effect on daily blood pressure profile, significantly reducing the load pressure and blood pressure variability. During treatment with the combination of enalapril and HCTZ combination of enalapril, HCTZ with amlodipine optimal daily profile of blood pressure after 12 weeks of reaching respectively 63.1% and 71.4% of patients. The treatment with combination of enalapril and HCTZ and adding of amlodipine is characterized by good endurance and high adherence to treatment.

  11. Twenty-four-hour plasma tryptophan concentrations and ratios are below normal in obese subjects and are not normalized by substantial weight reduction

    DEFF Research Database (Denmark)

    Breum, Leif; Rasmussen, Michael H; Hilsted, Jannik

    2003-01-01

    subjects. Blood samples were drawn frequently throughout the 24-h period. An insulin tolerance test was also used to determine whether weight loss altered the ability of insulin to modify plasma concentrations of tryptophan and of the other large neutral amino acids. RESULTS: Plasma tryptophan......BACKGROUND: Plasma tryptophan concentrations and the ratio of tryptophan to other large neutral amino acids (plasma tryptophan ratio) are reportedly low in obese subjects. The plasma tryptophan ratio predicts brain tryptophan uptake and serotonin production. If this ratio is low in obese subjects...... concentrations and ratios in obese subjects were low at all times; these effects persisted after weight reduction. Plasma concentrations of all the large neutral amino acids decreased during insulin infusion in all the groups. CONCLUSIONS: The low 24-h plasma tryptophan ratios in obese and formerly obese...

  12. Twenty four Hours Circadian Cortisol Profile in Shift Work Nurses

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    H Kakooei

    2009-04-01

    Full Text Available ABSTRACT: Introduction & Objective: It is well established that adrenal hormone cortisol has long been used in human psychobiological studies as a biological marker of circadian rhythm, stress, and anxiety. There is little information, however, about the interrelationships of night work, plasma cortisol levels in females’ nurses of the developing countries. The aim of the present study was to compare circadian cortisol profile between two groups of nurses with shift and permanent work in a Hospital affiliated to Shiraz University of Medical Sciences, Iran, between January 2006 to September 2008. Materials & Methods: In this experimental study, we examined the reproducibility of plasma cortisol levels during one month period in 34 shift work nurses and 10 permanent day shift works. We evaluated potential associations between night work and hormone levels, using current and shift work information for the health care shift workers. Results: The results clearly revealed that shift work significantly increased nighttime cortisol levels (34.93 μg/dl during night shift and decreased the peak levels of cortisol in the morning (39.03 μg/dl. During the work shift the plasma cortisol presented a decreased concentration in the morning and increasing levels (44.93 μg/dl by the end of the evening. In contrast , the permanent day work nurses, who had never worked at night shifts, showed a lowest secretion of cortisol during the first half of night time sleep (10.02 μg/dl , and a peak value of the cortisol after awakening at 07:00 h ( 59.75 μg/ml. We also observed a significant association between night work and increased levels of cortisol over the remaining of the day. Conclusion: It can be concluded that nurses with night shift work have an abnormal cortisol secretion profile. Shift work nurses on rotating night shifts seem to experience changes in hormones levels that may be associated with increased of circadian disorders risk observed among night – shift workers.

  13. Twenty-Four-Hour Ambulatory Blood Pressure Monitoring in Hypertension

    Science.gov (United States)

    2012-01-01

    Executive Summary Objective The objective of this health technology assessment was to determine the clinical effectiveness and cost-effectiveness of 24-hour ambulatory blood pressure monitoring (ABPM) for hypertension. Clinical Need: Condition and Target Population Hypertension occurs when either systolic blood pressure, the pressure in the artery when the heart contracts, or diastolic blood pressure, the pressure in the artery when the heart relaxes between beats, are consistently high. Blood pressure (BP) that is consistently more than 140/90 mmHg (systolic/diastolic) is considered high. A lower threshold, greater than 130/80 mmHg (systolic/diastolic), is set for individuals with diabetes or chronic kidney disease. In 2006 and 2007, the age-standardized incidence rate of diagnosed hypertension in Canada was 25.8 per 1,000 (450,000 individuals were newly diagnosed). During the same time period, 22.7% of adult Canadians were living with diagnosed hypertension. A smaller proportion of Canadians are unaware they have hypertension; therefore, the estimated number of Canadians affected by this disease may be higher. Diagnosis and management of hypertension are important, since elevated BP levels are related to the risk of cardiovascular disease, including stroke. In Canada in 2003, the costs to the health care system related to the diagnosis, treatment, and management of hypertension were over $2.3 billion (Cdn). Technology The 24-hour ABPM device consists of a standard inflatable cuff attached to a small computer weighing about 500 grams, which is worn over the shoulder or on a belt. The technology is noninvasive and fully automated. The device takes BP measurements every 15 to 30 minutes over a 24-to 28-hour time period, thus providing extended, continuous BP recordings even during a patient’s normal daily activities. Information on the multiple BP measurements can be downloaded to a computer. The main detection methods used by the device are auscultation and oscillometry. The device avoids some of the pitfalls of conventional office or clinic blood pressure monitoring (CBPM) using a cuff and mercury sphygmomanometer such as observer bias (the phenomenon of measurement error when the observer overemphasizes expected results) and white coat hypertension (the phenomenon of elevated BP when measured in the office or clinic but normal BP when measured outside of the medical setting). Research Questions Is there a difference in patient outcome and treatment protocol using 24-hour ABPM versus CBPM for uncomplicated hypertension? Is there a difference between the 2 technologies when white coat hypertension is taken into account? What is the cost-effectiveness and budget impact of 24-hour ABPM versus CBPM for uncomplicated hypertension? Research Methods Literature Search Search Strategy A literature search was performed on August 4, 2011 using OVID MEDLINE, MEDLINE In-Process and Other Non-Indexed Citations, EMBASE, the Cumulative Index to Nursing and Allied Health Literature (CINAHL), the Cochrane Library, and the International Agency for Health Technology Assessment (INAHTA) for studies published from January 1, 1997 to August 4, 2011. Abstracts were reviewed by a single reviewer. For those studies meeting the eligibility criteria, full-text articles were obtained. Reference lists were also examined for any additional relevant studies not identified through the search. Articles with unknown eligibility were reviewed with a second clinical epidemiologist and then a group of epidemiologists until consensus was established. The quality of evidence was assessed as high, moderate, low, or very low according to GRADE methodology. Inclusion Criteria English language articles; published between January 1, 1997 and August 4, 2011; adults aged 18 years of age or older; journal articles reporting on the effectiveness, cost-effectiveness, or safety for the comparison of interest; clearly described study design and methods; health technology assessments, systematic reviews, meta-analyses, or randomized controlled trials. Exclusion Criteria non-English papers; animal or in vitro studies; case reports, case series, or case-case studies; studies comparing different antihypertensive therapies and evaluating their antihypertensive effects using 24-hour ABPM; studies on home or self-monitoring of BP, and studies on automated office BP measurement; studies in high-risk subgroups (e.g. diabetes, pregnancy, kidney disease). Outcomes of Interest Patient Outcomes mortality: all cardiovascular events (e.g., myocardial infarction [MI], stroke); non-fatal: all cardiovascular events (e.g., MI, stroke); combined fatal and non-fatal: all cardiovascular events (e.g., MI, stroke); all non-cardiovascular events; control of BP (e.g. systolic and/or diastolic target level). Drug-Related Outcomes percentage of patients who show a reduction in, or stop, drug treatment; percentage of patients who begin multi-drug treatment; drug therapy use (e.g. number, intensity of drug use); drug-related adverse events. Quality of Evidence The quality of the body of evidence was assessed as high, moderate, low, or very low according to the GRADE Working Group criteria. As stated by the GRADE Working Group, the following definitions of quality were used in grading the quality of the evidence: High Further research is very unlikely to change confidence in the estimate of effect. Moderate Further research is likely to have an important impact on confidence in the estimate of effect and may change the estimate. Low Further research is very likely to have an important impact on confidence in the estimate of effect and is likely to change the estimate. Very Low Any estimate of effect is very uncertain. Summary of Findings Short-Term Follow-Up Studies (Length of Follow-Up of ≤ 1 Year) Based on very low quality of evidence, there is no difference between technologies for non-fatal cardiovascular events. Based on moderate quality of evidence, ABPM resulted in improved BP control among patients with sustained hypertension compared to CBPM. Based on low quality of evidence, ABPM resulted in hypertensive patients being more likely to stop antihypertensive therapy and less likely to proceed to multi-drug therapy compared to CBPM. Based on low quality of evidence, there is a beneficial effect of ABPM on the intensity of antihypertensive drug use compared to CBPM. Based on moderate quality of evidence, there is no difference between technologies in the number of antihypertensive drugs used. Based on low to very low quality of evidence, there is no difference between technologies in the risk for a drug-related adverse event or noncardiovascular event. Long-Term Follow-Up Study (Mean Length of Follow-Up of 5 Years) Based on moderate quality of evidence, there is a beneficial effect of ABPM on total combined cardiovascular events compared to CBPM. Based on low quality of evidence, there is a lack of a beneficial effect of ABPM on nonfatal cardiovascular events compared to CBPM; however, the lack of a beneficial effect is based on a borderline result. Based on low quality of evidence, there is no beneficial effect of ABPM on fatal cardiovascular events compared to CBPM. Based on low quality of evidence, there is no difference between technologies for the number of patients who began multi-drug therapy. Based on low quality of evidence, there is a beneficial effect of CBPM on control of BP compared to ABPM. This result is in the opposite direction than expected. Based on moderate quality of evidence, there is no difference between technologies in the risk for a drug-related adverse event. PMID:23074425

  14. The importance of cooling of urine samples for doping analysis

    NARCIS (Netherlands)

    Kuenen, J. Gijs; Konings, Wil N.

    2010-01-01

    Storing and transporting of urine samples for doping analysis, as performed by the anti-doping organizations associated with the World Anti-Doping Agency, does not include a specific protocol for cooled transport from the place of urine sampling to the doping laboratory, although low cost cooling fa

  15. The importance of cooling of urine samples for doping analysis

    NARCIS (Netherlands)

    Kuenen, J.G.; Konings, W.N.

    2009-01-01

    Storing and transporting of urine samples for doping analysis, as performed by the anti-doping organizations associated with the World Anti-Doping Agency, does not include a specific protocol for cooled transport from the place of urine sampling to the doping laboratory, although low cost cooling fa

  16. Tritium analysis of urine samples from the general Korean public.

    Science.gov (United States)

    Yoon, Seokwon; Ha, Wi-Ho; Lee, Seung-Sook

    2013-11-01

    The tritium concentrations of urine samples and the effective dose of the general Korean public were evaluated. To achieve accurate HTO analysis of urine samples, we established the optimal conditions for measuring the HTO content of urine samples. Urine samples from 50 Koreans who do not work at a nuclear facility were analyzed on the basis of the results. The average urine analysis result was 2.8 ±1 .4 Bq/L, and the range was 1.8-5.6 Bq/L. The measured values were lower than those reported for other countries. These results show that environmental factors and lifestyle differences are the main factors affecting the tritium level of the general public. © 2013 Elsevier Ltd. All rights reserved.

  17. Tracer techniques for urine volume determination and urine collection and sampling back-up system

    Science.gov (United States)

    Ramirez, R. V.

    1971-01-01

    The feasibility, functionality, and overall accuracy of the use of lithium were investigated as a chemical tracer in urine for providing a means of indirect determination of total urine volume by the atomic absorption spectrophotometry method. Experiments were conducted to investigate the parameters of instrumentation, tracer concentration, mixing times, and methods for incorporating the tracer material in the urine collection bag, and to refine and optimize the urine tracer technique to comply with the Skylab scheme and operational parameters of + or - 2% of volume error and + or - 1% accuracy of amount of tracer added to each container. In addition, a back-up method for urine collection and sampling system was developed and evaluated. This back-up method incorporates the tracer technique for volume determination in event of failure of the primary urine collection and preservation system. One chemical preservative was selected and evaluated as a contingency chemical preservative for the storage of urine in event of failure of the urine cooling system.

  18. Urine sampling techniques in symptomatic primary-care patients

    DEFF Research Database (Denmark)

    Holm, Anne; Aabenhus, Rune

    2016-01-01

    in primary care. The aim of this study was to determine the accuracy of urine culture from different sampling-techniques in symptomatic non-pregnant women in primary care. Methods: A systematic review was conducted by searching Medline and Embase for clinical studies conducted in primary care using......Background: Choice of urine sampling technique in urinary tract infection may impact diagnostic accuracy and thus lead to possible over- or undertreatment. Currently no evidencebased consensus exists regarding correct sampling technique of urine from women with symptoms of urinary tract infection...... seven studies investigating urine sampling technique in 1062 symptomatic patients in primary care. Mid-stream-clean-catch had a positive predictive value of 0.79 to 0.95 and a negative predictive value close to 1 compared to sterile techniques. Two randomized controlled trials found no difference...

  19. Efficacy of Urine Samples in Biioavailability Study of Ranitidine

    OpenAIRE

    Sima Sadray; Hosnieh Tajerzedeh; Afshin Mohajer; Ahmad Mirfazaelian Mohammad Reza Rouini

    2003-01-01

    Urinary excretion of ranitidine is known to be almost 70% of the intact drug , therefore this drug would be a good candidate for bioavailability studies using urine samples. In this study the bioequivalency of two marketed formulations using both urine and plasma samples were investigated. 'Ranitidine' 150 mg tablets (generic) and 'Zantac' 150 mg tablets were compared in a double blind crossover study using eight healthy male volunteers. A simple and rapid HPLC method was ...

  20. Efficacy of Urine Samples in Biioavailability Study of Ranitidine

    Directory of Open Access Journals (Sweden)

    Sima Sadray

    2003-08-01

    Full Text Available Urinary excretion of ranitidine is known to be almost 70% of the intact drug , therefore this drug would be a good candidate for bioavailability studies using urine samples. In this study the bioequivalency of two marketed formulations using both urine and plasma samples were investigated. 'Ranitidine' 150 mg tablets (generic and 'Zantac' 150 mg tablets were compared in a double blind crossover study using eight healthy male volunteers. A simple and rapid HPLC method was also developed to analyze the drug concentration in both urine and plasma. Double peak phenomenon, observed in plasma samples, was omitted when the urine samples were used. Bioavailability of the two formulations calculated from urinary data were not significantly different, whereas the plasma data were considerably different (based on Cmax & Tmax but not AUC. Pharmacokinetic parameters resulted from urine regarding the rate of the absorption (Tmax-ud, (dDu/dtmax, Ka-ud did not correlate well with their respective plasma parameters (Tmax, Cmax, Ka, whereas those of absorption extent and elimination rates (plasma AUC, K and urinary Du  were well correlated. It is concluded that the urine sampling which has advantages of easy sample collection and extraction could be used for determination of the extent of absorption and rate of the elimination of ranitidine, since similar parameters can be obtained with easier sample collection and extraction, whereas for determination of absorption rate, Cmax & Tmax plasma data are preferred. Key words: Ranitidine, Bioavailability, HPLC, Plasma, Urine.

  1. Reproducibility of urinary biomarkers in multiple 24-h urine samples.

    Science.gov (United States)

    Sun, Qi; Bertrand, Kimberly A; Franke, Adrian A; Rosner, Bernard; Curhan, Gary C; Willett, Walter C

    2017-01-01

    Limited knowledge regarding the reproducibility of biomarkers in 24-h urine samples has hindered the collection and use of the samples in epidemiologic studies. We aimed to evaluate the reproducibility of various markers in repeat 24-h urine samples. We calculated intraclass correlation coefficients (ICCs) of biomarkers measured in 24-h urine samples that were collected in 3168 participants in the NHS (Nurses' Health Study), NHSII (Nurses' Health Study II), and Health Professionals Follow-Up Study. In 742 women with 4 samples each collected over the course of 1 y, ICCs for sodium were 0.32 in the NHS and 0.34 in the NHSII. In 2439 men and women with 2 samples each collected over 1 wk to ≥1 mo, the ICCs ranged from 0.33 to 0.68 for sodium at various intervals between collections. The urinary excretion of potassium, calcium, magnesium, phosphate, sulfate, and other urinary markers showed generally higher reproducibility (ICCs >0.4). In 47 women with two 24-h urine samples, ICCs ranged from 0.15 (catechin) to 0.75 (enterolactone) for polyphenol metabolites. For phthalates, ICCs were generally ≤0.26 except for monobenzyl phthalate (ICC: 0.55), whereas the ICC was 0.39 for bisphenol A (BPA). We further estimated that, for the large majority of the biomarkers, the mean of three 24-h urine samples could provide a correlation of ≥0.8 with true long-term urinary excretion. These data suggest that the urinary excretion of various biomarkers, such as minerals, electrolytes, most polyphenols, and BPA, is reasonably reproducible in 24-h urine samples that are collected within a few days or ≤1 y. Our findings show that three 24-h samples are sufficient for the measurement of long-term exposure status in epidemiologic studies. © 2017 American Society for Nutrition.

  2. Miniaturized sample preparation method for determination of amphetamines in urine.

    Science.gov (United States)

    Nishida, Manami; Namera, Akira; Yashiki, Mikio; Kimura, Kojiro

    2004-07-16

    A simple and miniaturized sample preparation method for determination of amphetamines in urine was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). Urine was directly applied to the extraction column that was pre-packed with Extrelut and sodium carbonate. Amphetamine (AP) and methamphetamine (MA) in urine were adsorbed on the surface of Extrelut. AP and MA were then converted to a free base and derivatized to N-propoxycarbonyl derivatives using propylchloroformate on the column. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 100 and 102%, respectively. The calibration curves showed linearity in the range of 0.50-50 microg/mL for AP and MA in urine. When urine samples containing two different concentrations (0.50 and 5.0 microg/mL) of AP and MA were determined, the intra-day and inter-day coefficients of variation were 1.4-7.7%. This method was applied to 14 medico-legal cases of MA intoxication. The results were compared and a good agreement was obtained with a HPLC method.

  3. Optimization for Peptide Sample Preparation for Urine Peptidomics

    Energy Technology Data Exchange (ETDEWEB)

    Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan; Dai, Hong; Qian, Weijun; Camp, David G.; Sarwal, Minnie M.

    2014-02-25

    Analysis of native or endogenous peptides in biofluids can provide valuable insights into disease mechanisms. Furthermore, the detected peptides may also have utility as potential biomarkers for non-invasive monitoring of human diseases. The non-invasive nature of urine collection and the abundance of peptides in the urine makes analysis by high-throughput ‘peptidomics’ methods , an attractive approach for investigating the pathogenesis of renal disease. However, urine peptidomics methodologies can be problematic with regards to difficulties associated with sample preparation. The urine matrix can provide significant background interference in making the analytical measurements that it hampers both the identification of peptides and the depth of the peptidomics read when utilizing LC-MS based peptidome analysis. We report on a novel adaptation of the standard solid phase extraction (SPE) method to a modified SPE (mSPE) approach for improved peptide yield and analysis sensitivity with LC-MS based peptidomics in terms of time, cost, clogging of the LC-MS column, peptide yield, peptide quality, and number of peptides identified by each method. Expense and time requirements were comparable for both SPE and mSPE, but more interfering contaminants from the urine matrix were evident in the SPE preparations (e.g., clogging of the LC-MS columns, yellowish background coloration of prepared samples due to retained urobilin, lower peptide yields) when compared to the mSPE method. When we compared data from technical replicates of 4 runs, the mSPE method provided significantly improved efficiencies for the preparation of samples from urine (e.g., mSPE peptide identification 82% versus 18% with SPE; p = 8.92E-05). Additionally, peptide identifications, when applying the mSPE method, highlighted the biology of differential activation of urine peptidases during acute renal transplant rejection with distinct laddering of specific peptides, which was obscured for most proteins

  4. Natural radionuclides in urine- and faeces samples; Natuerliche Radionuklide in Urin- und Stuhlproben

    Energy Technology Data Exchange (ETDEWEB)

    Froning, M.; Burow, M.; Ennen, R.; Hoelters, A.; Laumen-Sentis, S.; Zoriy, M. [Forschungszentrum Juelich GmbH (Germany). Geschaeftsbereich Sicherheit und Strahlenschutz

    2016-07-01

    In interpreting of measurement data for incorporation monitoring by excretion samples a clear distinction between the natural intake and the fraction subjected due to occupational exposure should be performed. At the present only a few data about an excretion of primordial elements such as {sup 238}U, {sup 232}Th are available in the literature. In the following study actual data measured in urine and faeces will be presented and discussed.

  5. Microextraction Methods for Preconcentration of Aluminium in Urine Samples

    Directory of Open Access Journals (Sweden)

    Farzad Farajbakhsh, Mohammad Amjadi, Jamshid Manzoori, Mohammad R. Ardalan, Abolghasem Jouyban

    2016-07-01

    Full Text Available Background: Analysis of aluminium (Al in urine samples is required in management of a number of diseases including patients with renal failure. This work aimed to present dispersive liquid-liquid microextraction (DLLME and ultrasound-assisted emulsification microextraction (USAEME methods for the preconcentration of ultra-trace amount of aluminum in human urine prior to its determination by a graphite furnace atomic absorption spectrometry (GFAAS. Methods: The microextraction methods were based on the complex formation of Al3+ with 8-hydroxyquinoline. The effect of various experimental parameters on the efficiencies of the methods and their optimum values were studied. Results: Under the optimal conditions, the limits of detection for USAEME-GFAAS and DLLME-GFAAS were 0.19 and 0.30 ng mL−1, respectively and corresponding relative standard deviations (RSD, n=5 for the determination of 40 ng mL−1 Al3+ were 5.9% and 4.9%. Conclusion: Both methods could be successfully used to the analysis of ultra trace concentrations of Al in urine samples of dialysis patients.

  6. Excretion of arsenic (As) in urine of children, 7--11 years, exposed to elevated levels of As in the city water supply in Hermosillo, Sonora, Mexico

    Energy Technology Data Exchange (ETDEWEB)

    Wyatt, C.J.; Quiroga, V.L.; Acosta, R.T.O.; Mendez, R.O. [Centro de Investigaciones en Alimentacion y Desarrollo, Hermosillo (Mexico)

    1998-07-01

    Arsenic (As) is a common element in the environment with many industrial uses, but it also can be a contaminant in drinking water and present serious health concerns. Earlier studies on the quality of drinking water in the city of Hermosillo, Sonora, Mexico, showed high levels of As in water from wells located in the northern part of the city. Additionally a high positive correlation between the levels of Fluoride (F) and As in the same wells was found. Therefore, the objective of this study was to determine the excretion of As in children, 7--11 years of age, that had been exposed to elevated levels of As in their drinking water. Twenty-four-hour urine samples and a water sample taken directly in the home were collected from school age children living in two different areas with known high levels of As in their drinking water. A control group with normal levels of As in their water was also included.

  7. ISOLATION AND MOLECULAR IDENTIFICATION OF PATHOGENIC BACTERIA FROM URINE SAMPLE

    Directory of Open Access Journals (Sweden)

    Suhad A. Ibrahim

    2015-11-01

    Full Text Available Hospital environment is the major cause of variousinfections including cut and burn wounds. Urine Samples are one of the most common and devastating forms of trauma, exposing the immunosuppressed patients to early and serious infections. Faster detection of the causative Microbes and institution of proper therapy would help greatly in preventing septic complications. Recent advances in the field of Molecular Biology, including the amplification of genetic material by the Polymerase Chain Reaction (PCR technologies have led to faster and more reliable microbial detection methods. Results would help in early detection of causative organisms and treatment regimes in patients with burn wounds.

  8. Metabonomic responses in rat urine following subacute exposure to propoxur.

    Science.gov (United States)

    Liang, Yu-Jie; Wang, Hui-Ping; Yang, Lin; Li, Wei; Wu, Yi-Jun

    2012-06-01

    Metabolic profiling of urine from pesticide-treated rats was investigated by the nuclear magnetic resonance (NMR)-based metabonomic strategy. Twenty-four-hour urine samples of rats were collected after administration with propoxur at doses of 0.85, 1.70, and 8.51 mg/kg, respectively, for 28 consecutive days. Liver tissue was fixed and the histopathological alterations were examined. The results showed that propoxur at high dose induced liver histopathological injury. Metabonomic analysis demonstrated that the levels of creatine and taurine markedly increased together with slight elevation of hippurate, glucose, and amino acids in low- and medium-dose groups. However, concentrations of urinary lactate, acetate, acetone, succinate, citrate, and 2-oxoglutarate increased in high-dose group. All these results suggested that propoxur could inhibit liver function through altering the energy and lipid metabolism. These data also supported the contention that the NMR-based metabonomic approach represents a promising new technology for the development of pesticide toxicity screening and mechanism exploration.

  9. Twenty-four hour blood flow in the forefoot after reconstructive vascular surgery

    DEFF Research Database (Denmark)

    Jelnes, R

    1986-01-01

    Local blood flow in the forefoot (SBF) was measured continuously during 24 hours by 133xenon clearance technique in 10 patients prior to and at least 1 year after successful reconstructive vascular surgery for severe arterial insufficiency (mean: 18 months, range: 12-36). A group of 10 patients...... with normal peripheral circulation served as a control group. In spite of a considerable increase of the ankle/arm systolic blood pressure index--preoperative: 0.30 +/- 0.12, postoperative: 0.78 +/- 0.28 (mean +/- 1 SD)--the SBF decreased by 50% (p less than 0.001) following reconstructive vascular surgery...... are explained by the reappearance of peripheral vasoregulatory mechanisms. Postreconstructive hyperemia was evaluated by the same technique. The changes in SBF following surgery in the positions supine, awake and supine, asleep were found to be insignificant (0.80 less than p less than 0.90). It is concluded...

  10. Twenty-four hour urinary urea excretion and 9-year risk of hypertension: The PREVEND study

    NARCIS (Netherlands)

    Tielemans, S.M.A.J.; Geleijnse, J.M.; Baak, M.A. van; Engberink, M.F.; Brink, E.J.; Jong, P.E. de; Gansevoort, R.T.; Bakker, S.J.L.

    2013-01-01

    OBJECTIVES: It is not yet clear whether dietary protein could help maintaining a healthy blood pressure (BP). We investigated the association between total protein intake, estimated from 24-h urinary urea excretion, and incident hypertension in Dutch men and women. METHODS: We analyzed data of 3997

  11. Twenty-four-hour intraocular pressure patterns in a symptomatic patient after ab interno trabeculotomy surgery

    Directory of Open Access Journals (Sweden)

    Mansouri K

    2014-11-01

    Full Text Available Kaweh Mansouri,1 Felipe A Medeiros,2 Robert N Weinreb2 1Glaucoma Sector, Department of Ophthalmology, Geneva University Hospitals, Geneva, Switzerland; 2Hamilton Glaucoma Center and Department of Ophthalmology, University of California, San Diego, La Jolla, CA, USA Abstract: We report the results of repeated ambulatory continuous 24-hour intraocular pressure (IOP monitoring with a contact lens sensor (CLS in a glaucoma patient with ocular pain after ab interno trabeculotomy (Trabectome™ surgery. Our findings show that a combined prostaglandin–pilocarpine treatment reduced nighttime IOP peaks and relieved the patient’s symptoms. Keywords: 24-hour, Trabectome contact lens sensor, prostaglandin–pilocarpine treatment

  12. Twenty-four hour radioactive iodine uptake in 35 patients with amiodarone associated thyrotoxicosis

    Energy Technology Data Exchange (ETDEWEB)

    Martino, E.; Aghini-Lombardi, F.; Lippi, F.; Baschieri, L.; Safran, M.; Braverman, L.E.; Pinchera, A.

    1985-12-01

    Amiodarone associated thyrotoxicosis (AAT) occurs in approximately 10% of patients treated with this iodine rich drug in areas of mild iodine deficiency. The thyroid radioactive iodine uptake (RAIU) is usually undetectable or very low in iodine-induced thyrotoxicosis. In the present study, 35 patients with AAT were evaluated. Twelve patients had no thyroid abnormalities by physical exam and all had 24-hr RAIU less than or equal to 4%. In contrast, nine of 11 patients with AAT and diffuse goiters and eight of 12 patients with AAT and nodular goiters had RAIU values greater than 8%. In patients with AAT and goiter it appears possible that the thyroid fails to adapt normally to the excess iodide load, resulting in an inappropriately high RAIU in the presence of excess plasma iodine.

  13. Twenty-Four-Hour Mobility During Acute Hospitalization in Older Medical Patients

    DEFF Research Database (Denmark)

    Pedersen, Mette Merete; Bodilsen, Ann Christine; Petersen, Janne

    2013-01-01

    BACKGROUND: Inactivity during hospitalization in older medical patients may lead to functional decline. This study quantified 24-hour mobility, validated the accelerometers used, and assessed the daily level of basic mobility in acutely admitted older medical patients during their hospitalization...

  14. Twenty-four hour blood flow in the forefoot after reconstructive vascular surgery

    Energy Technology Data Exchange (ETDEWEB)

    Jelnes, R.

    1986-08-01

    Local blood flow in the forefoot (SBF) was measured continuously during 24 hours by 133xenon clearance technique in 10 patients prior to and at least 1 year after successful reconstructive vascular surgery for severe arterial insufficiency (mean: 18 months, range: 12-36). A group of 10 patients with normal peripheral circulation served as a control group. In spite of a considerable increase of the ankle/arm systolic blood pressure index--preoperative: 0.30 +/- 0.12, postoperative: 0.78 +/- 0.28 (mean +/- 1 SD)--the SBF decreased by 50% (p less than 0.001) following reconstructive vascular surgery during day activities. During sleep, however, SBF increased by 80% (p less than 0.001). The relative changes in SBF from day to night at the postoperative examination did not differ from that of the control group, i.e., the normal 24-hour blood flow pattern had been obtained. These changes in SBF are explained by the reappearance of peripheral vasoregulatory mechanisms. Postreconstructive hyperemia was evaluated by the same technique. The changes in SBF following surgery in the positions supine, awake and supine, asleep were found to be insignificant (0.80 less than p less than 0.90). It is concluded that the long-term postreconstructive hyperemia merely is a reflection of the normal 24-hour blood flow pattern.

  15. Twenty-four hour urinary urea excretion and 9-year risk of hypertension : the PREVEND study

    NARCIS (Netherlands)

    Tielemans, Susanne M. A. J.; Geleijnse, Johanna M.; van Baak, Marleen A.; Engberink, Marielle F.; Brink, Elizabeth J.; de Jong, Paul E.; Gansevoort, Ronald T.; Bakker, Stephan J. L.

    2013-01-01

    Objectives:It is not yet clear whether dietary protein could help maintaining a healthy blood pressure (BP). We investigated the association between total protein intake, estimated from 24-h urinary urea excretion, and incident hypertension in Dutch men and women.Methods:We analyzed data of 3997 men

  16. Twenty-four hour urinary urea excretion and 9-year risk of hypertension: the PREVEND study

    NARCIS (Netherlands)

    Tielemans, S.M.A.J.; Geleijnse, J.M.; Baak, van M.A.; Engberink, M.F.; Brink, E.J.; Jong, P.E.; Gansevoort, R.T.; Bakker, S.J.A.

    2013-01-01

    OBJECTIVES:: It is not yet clear whether dietary protein could help maintaining a healthy blood pressure (BP). We investigated the association between total protein intake, estimated from 24-h urinary urea excretion, and incident hypertension in Dutch men and women. METHODS:: We analyzed data of 399

  17. Twenty-four-hour ambulatory blood pressure in children with sleep-disordered breathing.

    Science.gov (United States)

    Amin, Raouf S; Carroll, John L; Jeffries, Jenny L; Grone, Charles; Bean, Judy A; Chini, Barbara; Bokulic, Ronald; Daniels, Stephen R

    2004-04-15

    Obstructive sleep apnea causes intermittent elevation of systemic blood pressure (BP) during sleep. To determine whether obstructive apnea in children has a tonic effect on diurnal BP, 24-hour ambulatory blood pressure was obtained from 60 children with mean age of 10.8 +/- 3.5 years. Thirty-nine children had obstructive apnea and 21 had primary snoring. Children with obstructive apnea had significantly greater mean BP variability during wakefulness and sleep, a higher night-to-day systolic BP, and a smaller nocturnal dipping of mean BP. Variability of mean arterial pressure during wakefulness was predicted by the desaturation, body mass, and arousal indices, whereas variability during sleep was predicted by apnea-hypopnea and body mass indices. Nocturnal BP dipping was predicted by the desaturation index. There were no significant differences in systolic, diastolic, or mean arterial BP during sleep between the groups. Diastolic BP during wakefulness was significantly different between the groups and correlated negatively with apnea-hypopnea index. We conclude that obstructive apnea in children is associated with 24-hour BP dysregulation and that, independent of obesity, the frequency of obstructive apnea, oxygen desaturation, and arousal contributes to abnormal BP control.

  18. Simpler spectrophotometric assay of paracetamol in tablets and urine samples

    Science.gov (United States)

    Sirajuddin; Khaskheli, Abdul Rauf; Shah, Afzal; Bhanger, Muhammad Iqbal; Niaz, Abdul; Mahesar, Sarfaraz

    2007-11-01

    A very fast, economical and simpler direct spectrophotometric method was investigated for paracetamol (PC) determination in aqueous medium without using any chemical reagents. The method is based on the photo-absorption of the analyte at 243 nm after dissolution in water. The change in structure of PC after addition of water was studied by comparing the corresponding FTIR spectra. Optimization studies were conducted by using a 5 μg ml -1 standard solution of the analyte. Various parameters studied include, time for stability and measurement of spectra, effect of HCl, NaOH, CH 3COOH and NH 3 for change in absorbance and shift in spectra, interference by some analgesic drugs and some polar solvents and temperature effect. After optimization, Beer's law was obeyed in the range of 0.3-20 μg ml -1 PC solution with a correlation coefficient of 0.9999 and detection limit of 0.1 μg ml -1. The newly developed method was successfully applied for PC determination in some locally available tablets and urine samples. The proposed method is very useful for quick analysis of various types of solid and liquid samples containing PC.

  19. Human papillomavirus detection from human immunodeficiency virus-infected Colombian women's paired urine and cervical samples.

    Science.gov (United States)

    Munoz, Marina; Camargo, Milena; Soto-De Leon, Sara C; Sanchez, Ricardo; Parra, Diana; Pineda, Andrea C; Sussmann, Otto; Perez-Prados, Antonio; Patarroyo, Manuel E; Patarroyo, Manuel A

    2013-01-01

    Infection, coinfection and type-specific human papillomavirus (HPV) distribution was evaluated in human immunodeficiency virus (HIV)-positive women from paired cervical and urine samples. Paired cervical and urine samples (n = 204) were taken from HIV-positive women for identifying HPV-DNA presence by using polymerase chain reaction (PCR) with three generic primer sets (GP5+/6+, MY09/11 and pU1M/2R). HPV-positive samples were typed for six high-risk HPV (HR-HPV) (HPV-16, -18, -31, -33, -45 and -58) and two low-risk (LR-HPV) (HPV-6/11) types. Agreement between paired sample results and diagnostic performance was evaluated. HPV infection prevalence was 70.6% in cervical and 63.2% in urine samples. HPV-16 was the most prevalent HPV type in both types of sample (66.7% in cervical samples and 62.0% in urine) followed by HPV-31(47.2%) in cervical samples and HPV-58 (35.7%) in urine samples. There was 55.4% coinfection (infection by more than one type of HPV) in cervical samples and 40.2% in urine samples. Abnormal Papanicolau smears were observed in 25.3% of the women, presenting significant association with HPV-DNA being identified in urine samples. There was poor agreement of cervical and urine sample results in generic and type-specific detection of HPV. Urine samples provided the best diagnosis when taking cytological findings as reference. In conclusion including urine samples could be a good strategy for ensuring adherence to screening programs aimed at reducing the impact of cervical cancer, since this sample is easy to obtain and showed good diagnostic performance.

  20. Human papillomavirus detection from human immunodeficiency virus-infected Colombian women's paired urine and cervical samples.

    Directory of Open Access Journals (Sweden)

    Marina Munoz

    Full Text Available Infection, coinfection and type-specific human papillomavirus (HPV distribution was evaluated in human immunodeficiency virus (HIV-positive women from paired cervical and urine samples. Paired cervical and urine samples (n = 204 were taken from HIV-positive women for identifying HPV-DNA presence by using polymerase chain reaction (PCR with three generic primer sets (GP5+/6+, MY09/11 and pU1M/2R. HPV-positive samples were typed for six high-risk HPV (HR-HPV (HPV-16, -18, -31, -33, -45 and -58 and two low-risk (LR-HPV (HPV-6/11 types. Agreement between paired sample results and diagnostic performance was evaluated. HPV infection prevalence was 70.6% in cervical and 63.2% in urine samples. HPV-16 was the most prevalent HPV type in both types of sample (66.7% in cervical samples and 62.0% in urine followed by HPV-31(47.2% in cervical samples and HPV-58 (35.7% in urine samples. There was 55.4% coinfection (infection by more than one type of HPV in cervical samples and 40.2% in urine samples. Abnormal Papanicolau smears were observed in 25.3% of the women, presenting significant association with HPV-DNA being identified in urine samples. There was poor agreement of cervical and urine sample results in generic and type-specific detection of HPV. Urine samples provided the best diagnosis when taking cytological findings as reference. In conclusion including urine samples could be a good strategy for ensuring adherence to screening programs aimed at reducing the impact of cervical cancer, since this sample is easy to obtain and showed good diagnostic performance.

  1. Estimating mean change in population salt intake using spot urine samples.

    Science.gov (United States)

    Petersen, Kristina S; Wu, Jason H Y; Webster, Jacqui; Grimes, Carley; Woodward, Mark; Nowson, Caryl A; Neal, Bruce

    2016-10-14

    : Spot urine samples are easier to collect than 24-h urine samples and have been used with estimating equations to derive the mean daily salt intake of a population. Whether equations using data from spot urine samples can also be used to estimate change in mean daily population salt intake over time is unknown. We compared estimates of change in mean daily population salt intake based upon 24-h urine collections with estimates derived using equations based on spot urine samples. : Paired and unpaired 24-h urine samples and spot urine samples were collected from individuals in two Australian populations, in 2011 and 2014. Estimates of change in daily mean population salt intake between 2011 and 2014 were obtained directly from the 24-h urine samples and by applying established estimating equations (Kawasaki, Tanaka, Mage, Toft, INTERSALT) to the data from spot urine samples. Differences between 2011 and 2014 were calculated using mixed models. : A total of 1000 participants provided a 24-h urine sample and a spot urine sample in 2011, and 1012 did so in 2014 (paired samples n = 870; unpaired samples n = 1142). The participants were community-dwelling individuals living in the State of Victoria or the town of Lithgow in the State of New South Wales, Australia, with a mean age of 55 years in 2011. The mean (95% confidence interval) difference in population salt intake between 2011 and 2014 determined from the 24-h urine samples was -0.48g/day (-0.74 to -0.21; P  0.058). Separate analysis of the unpaired and paired data showed that detection of change by the estimating equations was observed only in the paired data. : All the estimating equations based upon spot urine samples identified a similar change in daily salt intake to that detected by the 24-h urine samples. Methods based upon spot urine samples may provide an approach to measuring change in mean population salt intake, although further investigation in larger and more diverse population groups is

  2. Sample preparation for actinoides determination in urine; Probenvorbereitung fuer die Bestimmung von Actinoiden in Urin

    Energy Technology Data Exchange (ETDEWEB)

    Biehl, R.; Burow, M.; May, K.; Ostapczuk, P. [Abt. Sicherheit und Strahlenschutz, Forschungszentrum Juelich, Juelich (Germany)

    2002-07-01

    Mineralisation of up to 5 1 urine by UV-irradiation and destruction of urea by nitrous acid, produced by electrolysis were described. Phosphate precipitation following by coprecipitation on iron-tannin-complex increase the concentration of radionuclides 10{sup 4} times. Presented semi-automatic procedure minimise the digestion time and amount of used chemicals. (orig.)

  3. Contamination Rates of Three Urine-Sampling Methods to Assess Bacteriuria in Pregnant Women

    NARCIS (Netherlands)

    Schneeberger, Caroline; van den Heuvel, Edwin R.; Erwich, Jan Jaap H. M.; Stolk, Ronald P.; Visser, Caroline E.; Geerlings, Suzanne E.

    OBJECTIVE: To estimate and compare contamination rates of three different urine-sampling methods in pregnant women to assess bacteriuria. METHODS: In this cross-sectional study, 113 pregnant women collected three different midstream urine samples consecutively: morning (first void); midstream (void

  4. Urine concentrations of oral salbutamol in samples collected after intense exercise in endurance athletes

    DEFF Research Database (Denmark)

    Hostrup, Morten; Kalsen, Anders; Auchenberg, Michael

    2014-01-01

    of 1.020 g/mL compared with no adjustment. In conclusion, adjustment of urine samples to a USG of 1.020 g/mL decreases risk of false negative doping tests after administration of oral salbutamol. Adjusting urine samples for USG might be useful when evaluating urine concentrations of salbutamol...... by the Norwegian World Anti-doping Agency (WADA) laboratory. Adjustment of urine concentrations of salbutamol to a urine specific gravity (USG) of 1.020 g/mL was compared with no adjustment according to WADA's technical documents. We observed greater (P = 0.01) urine concentrations of salbutamol 4 h after...... in doping cases....

  5. Efficacy of 1% sodium fluoride as a preservative in urine samples containing glucose and Candida albicans.

    Science.gov (United States)

    Lough, P S; Fehn, R

    1993-03-01

    Whether urine samples used in forensic science DUI testing can be compromised by endogenous ethanol production is a recurrent and yet unresolved issue. This study first assessed unpreserved urine samples that were collected, processed, and analyzed repeatedly over 13 to 41 days using a standard gas chromatographic procedure for ethanol analysis. Despite extensive microbial growth, ethanol was not detected in any test sample. The extent of ethanol production in samples supplemented with glucose, Candida albicans, or both was determined to evaluate the potential for ethanol production in urine samples associated with pathological conditions such as urinary tract yeast infections and diabetes mellitus. Ethanol production under each of the above treatment conditions was assessed in the presence and absence of 1% sodium fluoride as a microbial suppressant. Mean ethanol concentrations were determined for unpreserved samples containing urine only (0.003 +/- 0.005 g%), urine plus yeast (0.006 +/- 0.009 g%) and urine plus glucose (0.067 +/- 0.070 g%). Unpreserved samples supplemented with both yeast and glucose attained mean ethanol concentrations of 0.164 +/- 0.057 g% (P urine samples indicates that false DUI convictions due to endogenous ethanol production are very unlikely. And while endogenous ethanol production is possible in the presence of both glucose and contaminating C. albicans, 1% sodium fluoride completely eliminated microbial fermentation.

  6. Urine concentrations of oral salbutamol in samples collected after intense exercise in endurance athletes.

    Science.gov (United States)

    Hostrup, Morten; Kalsen, Anders; Auchenberg, Michael; Rzeppa, Sebastian; Hemmersbach, Peter; Bangsbo, Jens; Backer, Vibeke

    2014-06-01

    Our objective was to investigate urine concentrations of 8 mg oral salbutamol in samples collected after intense exercise in endurance athletes. Nine male endurance athletes with a VO2max of 70.2 ± 5.9 mL/min/kg (mean ± SD) took part in the study. Two hours after administration of 8 mg oral salbutamol, subjects performed submaximal exercise for 15 min followed by two, 2-min exercise bouts at an intensity corresponding to 110% of VO2max and a bout to exhaustion at same intensity. Urine samples were collected 4, 8, and 12 h following administration of salbutamol. Samples were analyzed by the Norwegian World Anti-doping Agency (WADA) laboratory. Adjustment of urine concentrations of salbutamol to a urine specific gravity (USG) of 1.020 g/mL was compared with no adjustment according to WADA's technical documents. We observed greater (P = 0.01) urine concentrations of salbutamol 4 h after administration when samples were adjusted to a USG of 1.020 g/mL compared with no adjustment (3089 ± 911 vs. 1918 ± 1081 ng/mL). With the current urine decision limit of 1200 ng/mL for salbutamol on WADA's 2013 list of prohibited substances, fewer false negative urine samples were observed when adjusted to a USG of 1.020 g/mL compared with no adjustment. In conclusion, adjustment of urine samples to a USG of 1.020 g/mL decreases risk of false negative doping tests after administration of oral salbutamol. Adjusting urine samples for USG might be useful when evaluating urine concentrations of salbutamol in doping cases.

  7. Pomegranate juice ellagitannin metabolites are present in human plasma and some persist in urine for up to 48 hours.

    Science.gov (United States)

    Seeram, Navindra P; Henning, Susanne M; Zhang, Yanjun; Suchard, Marc; Li, Zhaoping; Heber, David

    2006-10-01

    Ellagitannins (ETs) from pomegranate juice (PJ) are reported to have numerous biological properties, but their absorption and metabolism in humans are poorly understood. To investigate the pharmacokinetics of pomegranate ETs, 18 healthy volunteers were given 180 mL of PJ concentrate, and blood samples were obtained for 6 h afterwards. Twenty-four-hour urine collections were obtained on the day before (-1), the day of (0), and the day after (+1) the study. Ellagic acid (EA) was detected in plasma of all subjects with a maximum concentration of 0.06 +/- 0.01 micromol/L, area under concentration time curve of 0.17 +/- 0.02 (micromol x h) x L(-1), time of maximum concentration of 0.98 +/- 0.06 h, and elimination half-life of 0.71 +/- 0.08 h. EA metabolites, including dimethylellagic acid glucuronide (DMEAG) and hydroxy-6H-benzopyran-6-one derivatives (urolithins), were also detected in plasma and urine in conjugated and free forms. DMEAG was found in the urine obtained from 15 of 18 subjects on d 0, but was not detected on d -1 or +1, demonstrating its potential as a biomarker of intake. Urolithin A-glucuronide was found in urine samples from 11 subjects on d 0 and in the urine from 16 subjects on d +1. Urolithin B-glucuronide was found in the urine of 3 subjects on d 0 and in the urine of 5 subjects on d +1. Urolithins, formed by intestinal bacteria, may contribute to the biological effects of PJ as they may persist in plasma and tissues and account for some of the health benefits noted after chronic PJ consumption. Whether genetic polymorphisms in EA-metabolizing enzymes (e.g., catechol-O-methyl transferase and glucuronosyl transferase) are related to variations in response to PJ remains to be established.

  8. Blue Chitin columns for the extraction of heterocyclic amines from urine samples

    DEFF Research Database (Denmark)

    Bang, J.; Frandsen, Henrik Lauritz; Skog, K.

    2004-01-01

    During normal cooking of meat, a class of mutagenic/carcinogenic compounds called heterocyclic amines is formed. Heterocyclic amines are rapidly absorbed and metabolised in the human body, and for estimation of the intake of heterocyclic amines, it is useful to determinate their levels in the urine....... Blue Chitin columns were used for the extraction and purification of heterocyclic amines from urine samples spiked with 14 different heterocyclic amines. The samples were analysed using LC-MS. The results show that Blue Chitin columns provide a straightforward and rapid means of extracting heterocyclic...... amines from urine samples, and that Blue Chitin column are also useful in the purification of urinary metabolites....

  9. Hypercalciuria, hyperoxaluria, and hypocitraturia screening from random urine samples in patients with calcium lithiasis.

    Science.gov (United States)

    Arrabal-Polo, Miguel Angel; Arias-Santiago, Salvador; Girón-Prieto, María Sierra; Abad-Menor, Felix; López-Carmona Pintado, Fernando; Zuluaga-Gomez, Armando; Arrabal-Martin, Miguel

    2012-10-01

    Calcium lithiasis is the most frequently diagnosed renal lithiasis and is associated with a high percentage of patients with metabolic disorders, such as hypercalciuria, hypocitraturia, and hyperoxaluria. The present study included 50 patients with recurrent calcium lithiasis. We conducted a random urine test during nocturnal fasting and a 24-h urine test, and examined calcium, oxalate, and citrate. A study of the linear correlation between the metabolites was performed, and the receiver operator characteristic (ROC) curves were analyzed in the random urine samples to determine the cutoff values for hypercalciuria (excretion greater than 200 mg), hyperoxaluria (excretion greater than 40 mg), and hypocitraturia (excretion less than 320 mg) in the 24-h urine. Linear relationships were observed between the calcium levels in the random and 24-h urine samples (R = 0.717, p = 0.0001), the oxalate levels in the random and 24-h urine samples (R = 0.838, p = 0.0001), and the citrate levels in the random and 24-h urine samples (R = 0.799, p = 0.0001). After obtaining the ROC curves, we observed that more than 10.15 mg/dl of random calcium and more than 16.45 mg/l of random oxalate were indicative of hypercalciuria and hyperoxaluria, respectively, in the 24-h urine. In addition, we found that the presence of less than 183 mg/l of random citrate was indicative of the presence of hypocitraturia in the 24-h urine. Using the proposed values, screening for hypercalciuria, hyperoxaluria, and hypocitraturia can be performed with a random urine sample during fasting with an overall sensitivity greater than 86%.

  10. EVALUATION OF DISPOSABLE DIAPERS FOR QUANTATIVE MEASUREMENTS OF PESTICIDE METABOLITES AND CREATININE IN URINE SAMPLES

    Science.gov (United States)

    This project consisted of a laboratory study to evaluate an extraction and analysis method for quantifying biomarkers of pesticide exposure and creatinine in urine samples collected with commercially-available disposable diapers. For large exposure studies, such as the National ...

  11. Lead Quantification in Urine Samples of Athletes by Coupling DLLME with UV-Vis Spectrophotometry.

    Science.gov (United States)

    Faraji, Hakim; Helalizadeh, Masoumeh

    2017-04-01

    Urine lead level is one of the most employed measures of lead exposure and risk. The urine samples used in this study were obtained from ten healthy male cyclists. Dispersive liquid-liquid microextraction combined with ultraviolet and visible spectrophotometry was utilized for preconcentration, extraction, and determination of lead in urine samples. Optimization of the independent variables was carried out based on chemometric methods in three steps. According to the screening and optimization study, 133 μL of CCl4 (extracting solvent), 1.34 mL ethanol (dispersing solvent), pH 2.0, 0.00 % of salt, and 0.1 % O,O-diethyl dithiophosphoric (chelating agent) were used as the optimum independent variables for microextraction and determination of lead. Under the optimized conditions, R (2) was 0.9991, and linearity range was 0.01-100 μg L(-1). Precision was evaluated in terms of repeatability and intermediate precision, with relative standard deviations being urine samples of cyclists as real samples and it was confirmed. The relative error of ≤5 % was considered significant in the method specificity study. The lead concentration mean for the cyclists was 3.79 μg L(-1) in urine samples. As a result, the proposed method is a robust technique to quantify lead concentrations higher than 11.6 ng L(-1) in urine samples.

  12. A Comparison of 4- and 24-Hour Urine Samples for the Diagnosis of Proteinuria in Pregnancy

    Directory of Open Access Journals (Sweden)

    Afsane Amirabi

    2011-09-01

    Full Text Available Background: Preeclampsia is a serious complication of pregnancy, and it is vital to diagnosis the condition as early as possible. Proteinuria is an important symptom of preeclampsia, and repeated urine analysis to screen for the condition is part of the standard antenatal care. The purpose of this study was to determine the correlation between 4- and 24-hour urine total protein values to examine whether the 4-hour urine samples could be used for the diagnosis of proteinuria in hypertensive disorders of pregnancy. Methods: A cross-sectional study was performed on 110 pregnant (after gestational week 20 of pregnancy patients who were hypertensive (blood pressure ≥140/90 mmHg and had proteinuria as defined by positive urinary protein of at least 1+ in dipstick. Patients' urine samples were collected over 24 hours; the first 4 hours were collected separately from the next 20-hours. Patients, who did not collect the 24-hour urine, were excluded from the study. One hundred patients met the criteria, and were included in the study. The urine volume, total protein and creatinine levels of 4- and 24-hours samples were measured. The correlation between 4-hour and 24-hour samples was examined using Pearson correlation test. Results: Of the 100 patients, 42 had no proteinuria, 44 had mild proteinuria, and 14 had severe proteinuria. The urine protein values of 4-hour samples correlated with those of the 24-hours samples for patients with mild and severe forms of the disease (P<0.001, r=0.86. Conclusion: This study showed there was a correlation between 4-hour and 24-hour urine proteins. The finding indicates that a random 4-hour sample might be used for the initial assessment of proteinuria

  13. Characterization of Bacterial Strains Isolated Through Microbial Profiling of Urine Samples

    Directory of Open Access Journals (Sweden)

    Poulomi Nandy

    2007-01-01

    Full Text Available The present study was conducted to determine the microbial profile in urine samples. Differential and selective chromogenic culture media were used for the rapid detection, identification and enumeration of urinary tract pathogens namely, E. coli, Pseudomonas aeruginosa, Klebsiella pneumoniae, Staphylococcus aureus, Enterococcus faecalis, Proteus mirabilis. Urine samples of normal healthy individuals as well as patients with Urinary Tract Infection (UTI were screened on hicrome agar plates. The cultivable bacteria present in urine were isolated based on chromogenic detection. Antibiotic sensitivity assay, morphological characterization and biochemical tests, namely protease, oxidase, catalase, lipase, DNase and lecithinase assay were performed with the 15 isolates obtained from urine samples. The molecular analyses of the isolates were done through partial sequencing of the 16SrDNA gene; six of them were found to be novel and submitted in GenBank under the accession numbers EF644491-96. Phylogenetic tree of the isolates were constructed by neighbour joining method.

  14. Urine storage under refrigeration preserves the sample in chemical, cellularity and bacteriuria analysis of ACS

    Directory of Open Access Journals (Sweden)

    Karen Cristina Barcellos Ribeiro

    2013-12-01

    Full Text Available INTRODUCTION: The analysis of urine abnormal constituents and sediment (ACS comprises tests of great diagnostic and prognostic value in clinical practice. When the analysis of ACS cannot be performed within two hours after collection, the sample must be preserved in order to avoid pre-analytical interferences. Refrigeration is the most applied technique due to its cost effectiveness. Moreover, it presents fewer inconveniences when compared to chemical preservation. However, changes in ACS may also occur in samples under refrigeration. OBJECTIVE: To analyze the influence of refrigeration at 2 to 8ºC on the storage of urine samples within 24 hours. MATERIAL AND METHOD: A total of 80 urine samples were selected from patients admitted at Universidade Federal de Juiz de Fora (UFJF university hospital, which were tested for ACS at room temperature and stored under refrigeration for 6, 12 and 24 hours. RESULTS: The results showed that refrigeration proved to be effective when compared to samples kept at room temperature, inasmuch as the physical, chemical, microbial and cellularity features were preserved. Nevertheless, crystalluria was present after a 6- hour storage period. CONCLUSION: The tests revealed that cooling preserved cellularity and chemical characteristics of urine samples for up to 12 hours. Nonetheless, the precipitation of crystals was evident in this storage method. Thus, the possible consequences of storing urine samples for ACS test under these conditions should be included in the analysis report.

  15. Urine sampling techniques in symptomatic primary-care patients: a diagnostic accuracy review.

    Science.gov (United States)

    Holm, Anne; Aabenhus, Rune

    2016-06-08

    Choice of urine sampling technique in urinary tract infection may impact diagnostic accuracy and thus lead to possible over- or undertreatment. Currently no evidencebased consensus exists regarding correct sampling technique of urine from women with symptoms of urinary tract infection in primary care. The aim of this study was to determine the accuracy of urine culture from different sampling-techniques in symptomatic non-pregnant women in primary care. A systematic review was conducted by searching Medline and Embase for clinical studies conducted in primary care using a randomized or paired design to compare the result of urine culture obtained with two or more collection techniques in adult, female, non-pregnant patients with symptoms of urinary tract infection. We evaluated quality of the studies and compared accuracy based on dichotomized outcomes. We included seven studies investigating urine sampling technique in 1062 symptomatic patients in primary care. Mid-stream-clean-catch had a positive predictive value of 0.79 to 0.95 and a negative predictive value close to 1 compared to sterile techniques. Two randomized controlled trials found no difference in infection rate between mid-stream-clean-catch, mid-stream-urine and random samples. At present, no evidence suggests that sampling technique affects the accuracy of the microbiological diagnosis in non-pregnant women with symptoms of urinary tract infection in primary care. However, the evidence presented is in-direct and the difference between mid-stream-clean-catch, mid-stream-urine and random samples remains to be investigated in a paired design to verify the present findings.

  16. Dried urine spots - A novel sampling technique for comprehensive LC-MS(n) drug screening.

    Science.gov (United States)

    Michely, Julian A; Meyer, Markus R; Maurer, Hans H

    2017-08-22

    Dried matrix spot (DMS) technique as alternative sampling strategy, especially dried urine spots (DUS), might be an alternative for drug screening. So far only particular drugs or drug classes were covered in DMS screenings. Therefore, workup of DUS for a broad comprehensive library-based LC-MS(n) screening was developed. It consisted of enzymatic on-spot deconjugation followed by liquid extraction and LC-MS(n) analysis. This workup was compared to established urine precipitation (UP) and validated according to international guidelines for qualitative approaches, using exemplary compounds of several drug classes (antidepressants, benzodiazepines, cardiovascular drugs, neuroleptics, opioids, stimulants, etc.) with a broad range of (physico-)chemical properties and chromatographic behaviors. On-spot conjugate cleavage and liquid extraction was sufficient for most compounds and the validation results comparable to those obtained after simple UP. For demonstrating the applicability, 103 authentic urine samples, six rat urine samples after low dose substance administrations, and two proficiency tests for systematic toxicological urinalysis were worked up with the new DUS approach or by UP without or with conjugate cleavage. In the authentic urine samples, 112 different drugs out of 43 categories plus metabolites were identified via the used LC-MS(n) library. With the new DUS approach, 5% less positive hits could be found compared to the UP approach and 15% less than the latter after conjugate cleavage. The differences should be caused mainly by smaller urine volumes used for DUS. In the two proficiency tests, all 15 drugs could be detected. Unfortunately, all three approaches were not able to detect very low-dosed substances in rat urine samples. However, they could be detected using a more sensitive LC-high resolution-MS/MS approach showing that the DUS workup was also suitable for those. In conclusion, DUS might be an alternative sampling technique for comprehensive

  17. Direct Susceptibility testing of Urine samples after 6, 9 and 16 hours incubation

    DEFF Research Database (Denmark)

    Ghatian, Khaled; Littauer, Pia; Llado, Minna Fyhn Lykke

    2015-01-01

    Objectives: At present, susceptibility testing of infective bacteria from urine samples, according to EUCAST, is interpretation of zones after 16 hours of incubation. Using a semi-automated sample processing, the Kiestra (BD) system, to incubate of the agar plates and digital image processing...... testing on urine samples. Methods: In total 675 consecutive urine samples from out-patients, were inoculated directly, according to our laboratory standard, as 10µL on each part of a bi-plate (oxoid chomogene agar and 5% horse blood-agar) and 10µL on a MH plate for resistance testing, using an Inoqula...... (Kiestra-BD). The plates were photographed at 6, 9 and 16 hours after incubation. As a gold standard, the susceptibility test was performed according to EUCAST, as a secondary susceptibility testing, for colonies identified on the biplates, and read after 16 hours incubation.The disks used (Oxoid, Termo...

  18. The method of urine sampling is not a valid predictor for vesicoureteral reflux in children after febrile urinary tract infections.

    Science.gov (United States)

    Haid, Bernhard; Roesch, Judith; Strasser, Christa; Oswald, Josef

    2017-03-16

    The likelihood of detecting vesicoureteral reflux (VUR) after febrile urinary tract infections (UTI) in children logically should correlate with the correct diagnosis of the UTI. Beneath the unspecific symptoms of fever urine analysis is the main diagnostic criterion for the exact diagnosis of febrile UTIs in children. Use of inadequate urine sampling techniques during diagnosis may lead to impaired accuracy in UTI diagnosis. This could lead to the assumption that children, having diagnosed their UTI by the use of possibly inadequate urine sampling techniques should not be evaluated as consequently compared to those, where the diagnosis relied on sterile urine sampling techniques. We hypothesized that children with possibly contaminated urine samples during the initial diagnosis may show a lower rate of VUR in subsequent VCUGs because of a wrong diagnosis initially compared to children, where accurate urine sampling techniques were used. Between 2009 and 2014, a total of 555 patients underwent a primary VCUG at our department indicated because of febrile UTIs. Patients with urine collection methods other than bag urine and catheter/suprapubic aspiration (SPA) were excluded from this study (mid-stream urine, potty urine, n = 149). We evaluated 402 patients (male/female 131/271, mean age 1.91 years), VUR rates and grades were compared between patients where urine was sampled by the use of a urine bag only at the time of diagnosis (n = 296, 73.6%) and those where sterile urine sampling (catheter, suprapubic puncture) was performed (n = 106, 26.3%). 4 patients were excluded due to equivocal data on urine sampling. VUR rate in children after sterile urine sampling using a catheter or SPA accounted to 31.1%. In those where urine samples acquired by the use of urine bags were used, 33.7% showed VUR on subsequent VCUG (p = 0.718). There were no significant differences as to VUR grades or gender, although VUR was much more commonly diagnosed in female patients (37

  19. Improving mid stream urine sampling: reducing labelling error and laboratory rejection.

    Science.gov (United States)

    Jakes, Adam; McCue, Eleanor; Cracknell, Alison

    2014-01-01

    A urine sample is vital in older patients with pyrexia or acute confusion, and commonly directs clinicians towards a source of infection. Not only can the organism be identified, but sensitivities to antibiotics can also guide prescribing. A high number of urine samples were not being processed on the medicine for older people wards at St. James's Hospital due to incomplete hand-written request forms not complying with trust policy. Previous attempts to re-educate staff had failed to improve acceptance rates. Rejected samples delay diagnosis, identification of organisms and subsequent sensitivities, as well as increasing staff workload. A total of 72 urine samples were audited from our wards in March 2013; 12 (17%) rejected. Clinicians were notified of rejected samples within one to four days. An electronic-requesting system was implemented in April 2013. Once implemented, a further two data collection cycles of 72 urine samples were completed from the same wards. In December 2013, 55 (76%) were electronically requested and 17 (24%) hand-written. Four (5%) samples were rejected and were all hand-written. In August 2014, 61 (85%) were electronically requested and 11 (15%) hand-written. No samples were rejected. The electronic-requesting system has effectively reduced the number of rejected urine samples. No electronically requested samples were rejected, therefore 100% sample acceptance is achievable. It is more effective than re-educating staff alone and ensures requests meet trust policy. Clinicians were notified of a samples rejection after one to four days. By this time patients may have started antibiotic therapy, decreasing the likelihood of isolating the causative organism in subsequent samples. All urine samples requested must meet a high standard and comply with trust policy in order to be processed. An electronic-requesting system removes errors of omission and ensures policy compliance, ultimately leading to improved patient care. Now our processes are

  20. Impact of cleaning before obtaining midstream urine samples from children

    DEFF Research Database (Denmark)

    Lytzen, Rebekka; Knudsen, Jenny Dahl; Ladelund, Steen

    2014-01-01

    24 h. In 2004-2006 ("cleaning period"), 523 children were cleaned before obtaining two MSUs, contrary to the 1,335 children included in 2008-2010 ("non-cleaning period"). Significant bacteriuria was defined as at least 10,000 colony-forming units/ml of the same uropathogenic bacterium in two MSUs...... in monoculture. Contamination was defined as all other microbiological findings. RESULTS: The procedure of no cleaning before sampling increased the risk of contamination in 0-9.9-year-old children from 43% to 49% (p = 0.034); and specifically in 0-9.9-year-old girls, the risk of contamination increased from 47...... than ten years of age is recommended to minimise the risk of contamination. Cleaning was without effect on children aged 10-15 years. FUNDING: not relevant. TRIAL REGISTRATION: not relevant....

  1. A salting out and resin procedure for extracting Schistosoma mansoni DNA from human urine samples

    Directory of Open Access Journals (Sweden)

    Rodrigues Nilton B

    2010-04-01

    Full Text Available Abstract Background In this paper a simple and cheap salting out and resin (InstaGene matrix® resin - BioRad DNA extraction method from urine for PCR assays is introduced. The DNA of the fluke Schistosoma mansoni was chosen as the target since schistosomiasis lacks a suitable diagnostic tool which is sensitive enough to detect low worm burden. It is well known that the PCR technique provides high sensitivity and specificity in detecting parasite DNA. Therefore it is of paramount importance to take advantage of its excellent performance by providing a simple to handle and reliable DNA extraction procedure, which permits the diagnosis of the disease in easily obtainable urine samples. Findings The description of the extraction procedure is given. This extraction procedure was tested for reproducibility and efficiency in artificially contaminated human urine samples. The reproducibility reached 100%, showing positive results in 5 assay repetitions of 5 tested samples each containing 20 ng DNA/5 ml. The efficiency of the extraction procedure was also evaluated in a serial dilution of the original 20 ng DNA/5 ml sample. Detectable DNA was extracted when it was at a concentration of 1.28 pg DNA/mL, revealing the high efficiency of this procedure. Conclusions This methodology represents a promising tool for schistosomiasis diagnosis utilizing a bio-molecular technique in urine samples which is now ready to be tested under field conditions and may be applicable to the diagnosis of other parasitic diseases.

  2. Metabolomic analysis of urine samples by UHPLC-QTOF-MS: Impact of normalization strategies.

    Science.gov (United States)

    Gagnebin, Yoric; Tonoli, David; Lescuyer, Pierre; Ponte, Belen; de Seigneux, Sophie; Martin, Pierre-Yves; Schappler, Julie; Boccard, Julien; Rudaz, Serge

    2017-02-22

    Among the various biological matrices used in metabolomics, urine is a biofluid of major interest because of its non-invasive collection and its availability in large quantities. However, significant sources of variability in urine metabolomics based on UHPLC-MS are related to the analytical drift and variation of the sample concentration, thus requiring normalization. A sequential normalization strategy was developed to remove these detrimental effects, including: (i) pre-acquisition sample normalization by individual dilution factors to narrow the concentration range and to standardize the analytical conditions, (ii) post-acquisition data normalization by quality control-based robust LOESS signal correction (QC-RLSC) to correct for potential analytical drift, and (iii) post-acquisition data normalization by MS total useful signal (MSTUS) or probabilistic quotient normalization (PQN) to prevent the impact of concentration variability. This generic strategy was performed with urine samples from healthy individuals and was further implemented in the context of a clinical study to detect alterations in urine metabolomic profiles due to kidney failure. In the case of kidney failure, the relation between creatinine/osmolality and the sample concentration is modified, and relying only on these measurements for normalization could be highly detrimental. The sequential normalization strategy was demonstrated to significantly improve patient stratification by decreasing the unwanted variability and thus enhancing data quality.

  3. Is aging raw cattle urine efficient for sampling Anopheles arabiensis Patton?

    NARCIS (Netherlands)

    Mahande, A.M.; Mwang'onde, B.J.; Msangi, S.; Kimaro, E.; Mnyone, L.L.; Mazigo, H.D.; Mahande, M.J.; Kweka, E.J.

    2010-01-01

    Background: To ensure sustainable routine surveillance of mosquito vectors, simple, effective and ethically acceptable tools are required. As a part of that, we evaluated the efficiency of resting boxes baited with fresh and aging cattle urine for indoor and outdoor sampling of An. arabiensis in the

  4. The Determination of Polyethylene Glycol in Untreated Urine Samples by High Performance Liquid Chromatography for Intestinal Permeability Studies

    DEFF Research Database (Denmark)

    Larsen, Elfinn; Pedersen, Walther Batsberg; Philipsen, E.

    1985-01-01

    Polyethylene glycol in urine samples has been investigated by high performance liquid chromatography. The molecular weights ranged from 634 to 1338. The urine samples were applied to the chromatographic system without any pre-treatment. For samples with a concentration of 0.2% polyethylene glycol...

  5. Reliable Quantification of the Potential for Equations Based on Spot Urine Samples to Estimate Population Salt Intake

    DEFF Research Database (Denmark)

    Huang, Liping; Crino, Michelle; Wu, Jason Hy

    2016-01-01

    BACKGROUND: Methods based on spot urine samples (a single sample at one time-point) have been identified as a possible alternative approach to 24-hour urine samples for determining mean population salt intake. OBJECTIVE: The aim of this study is to identify a reliable method for estimating mean p...

  6. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier

    2013-01-01

    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  7. Reproducibility of NMR analysis of urine samples: impact of sample preparation, storage conditions, and animal health status.

    Science.gov (United States)

    Schreier, Christina; Kremer, Werner; Huber, Fritz; Neumann, Sindy; Pagel, Philipp; Lienemann, Kai; Pestel, Sabine

    2013-01-01

    Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining (1)H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after (1)H NMR spectroscopy. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at -20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  8. HPLC determination of ciprofloxacin, cloxacillin, and ibuprofen drugs in human urine samples.

    Science.gov (United States)

    Espinosa-Mansilla, Anunciación; Muñoz de la Peña, Arsenio; González Gómez, David; Cañada-Cañada, Florentina

    2006-08-01

    This paper reports, for the first time, a liquid chromatographic method for the simultaneous determination of three frequently co-administered active principles, two antibiotics, ciprofloxacin (CIPRO) and cloxacillin (CLOXA) belonging to the fluoroquinolones and beta-lactam families, respectively, and ibuprofen (IBU), a non-steroidal anti-inflammatory drug. The chromatographic separation was performed on a C-18 analytical column, using isocratic elution with methanol-acetonitrile-pH 3 formate buffer (CT = 0.1 M) (15:12:73, v/v/v) for 3 min and, after that, a linear gradient with methanol-acetonitrile (88:12, v/v) for 8 min. Several absorption spectra were obtained for each peak using a DAD detector. Chromatograms at the maximum absorption wavelength for each analyte, 220 nm for both IBU and CLOXA, and 280 nm for CIPRO were selected as the most suitable. The proposed chromatographic method requires about 15 min per sample. The presence of a urine background was tested and no interference was found. The method was satisfactorily applied to the determination of CIPRO, CLOXA, and IBU, in fortified urine, and in urine samples from a patient undergoing treatment with these three active principles, among others. Limits of quantification in urine were 1.00, 1.70, and 2.87 microg/mL for CIPRO, CLOXA, and IBU, respectively.

  9. Direct Agglutination Test and Enzyme Linked Immunosorbent Assay with Urine Samples for the Diagnosis of Visceral Leishma-niasis

    Directory of Open Access Journals (Sweden)

    Sarkari B

    2007-07-01

    Full Text Available Background: Visceral leishmaniasis (VL or Kala azar is an infectious disease caused by various species of Leishmania parasites. The aim of this study was to detect and compare the presence of anti-Leishmania antibodies in the urine of vis-ceral leishmaniasis patients using ELISA and DAT methods."nMethods: A total of 30 urine samples were collected from VL patients referred to Shiraz (southeast of Iran hospitals. Moreover 31 urine samples were collected from healthy individuals and patients with other diseases such as malaria, brucellosis, hydatidosis and cutaneous leishmaniasis. Collected samples were examined to detect anti-Leishmania antibod-ies in urine, using ELISA and DAT."nResults: Anti-Leishmania antibody was detected in urine of 18 out of 30 (60% VL patients by DAT while ELISA detected anti-Leishmania antibodies in urine of 28 out of 30 (93.3% of VL cases. Sensitivity and specificity of urine-based DAT was 60% and 83.9%, respectively while sensitivity and specificity of urine-based ELISA were 93.3% and 93.5%, corre-spondingly. "nConclusion: Urine-based DAT and ELISA have a reasonable specificity and sensitivity in diagnosis of VL. Accordingly, urine-based ELISA might be a suitable alternative for serum based assays for diagnosis of VL.

  10. Comparison of uncertainties related to standardization of urine samples with volume and creatinine concentration

    DEFF Research Database (Denmark)

    Garde, Anne Helene; Hansen, Ase Marie; Kristiansen, Jesper;

    2004-01-01

    When measuring biomarkers in urine, volume (and time) or concentration of creatinine are both accepted methods of standardization for diuresis. Both types of standardization contribute uncertainty to the final result. The aim of the present paper was to compare the uncertainty introduced when using...... that the uncertainty associated with creatinine standardization (19-35%) was higher than the uncertainty related to volume standardization (up to 10%, when not correcting for deviations from 24 h) for 24 h urine samples. However, volume standardization introduced an average bias of 4% due to missed volumes...... in population studies. When studying a single 24 h sample from one individual, there was a 15-20% risk that the sample was incomplete. In this case a bias of approximately 25% was introduced when using volume standardization, whereas the uncertainty related to creatinine standardization was independent...

  11. A follow-up urine sample has limited value after treatment for urinary tract infection in children

    DEFF Research Database (Denmark)

    Lytzen, Rebekka; Kaalund-Jørgensen, Kristine; Ahmed, Akhlaq

    2015-01-01

    INTRODUCTION: A routine follow-up urine sample (FUS) in the form of a midstream urine sample (MSU) is recommended after treatment for urinary tract infection (UTI) according to the Danish Paediatric Society (DPS) and "Lægehåndbogen" published by Danish Regions. We studied the effect of FUS...

  12. A follow-up urine sample has limited value after treatment for urinary tract infection in children

    DEFF Research Database (Denmark)

    Lytzen, Rebekka; Kaalund-Jørgensen, Kristine; Ahmed, Akhlaq

    2015-01-01

    INTRODUCTION: A routine follow-up urine sample (FUS) in the form of a midstream urine sample (MSU) is recommended after treatment for urinary tract infection (UTI) according to the Danish Paediatric Society (DPS) and "Lægehåndbogen" published by Danish Regions. We studied the effect of FUS...

  13. Optimized preparation of urine samples for two-dimensional electrophoresis and initial application to patient samples

    DEFF Research Database (Denmark)

    Lafitte, Daniel; Dussol, Bertrand; Andersen, Søren;

    2002-01-01

    protein excretion patterns of 49 healthy men and 4 patients with renal disease were obtained by 2D electrophoresis. Silver nitrate stained protein spots were identified by mass spectrometry. RESULTS: Reproductive 2D gels identified 5 classes of proteins systematically found in healthy subjects...... was constant over time and reveal for the first time the relative abundance of albumin fragments in healthy subjects' urine. The profiles of the 4 patients, were specific of their renal disease....

  14. Optimization of a Pre-MEKC Separation SPE Procedure for Steroid Molecules in Human Urine Samples

    Directory of Open Access Journals (Sweden)

    Ilona Olędzka

    2013-11-01

    Full Text Available Many steroid hormones can be considered as potential biomarkers and their determination in body fluids can create opportunities for the rapid diagnosis of many diseases and disorders of the human body. Most existing methods for the determination of steroids are usually time- and labor-consuming and quite costly. Therefore, the aim of analytical laboratories is to develop a new, relatively low-cost and rapid implementation methodology for their determination in biological samples. Due to the fact that there is little literature data on concentrations of steroid hormones in urine samples, we have made attempts at the electrophoretic determination of these compounds. For this purpose, an extraction procedure for the optimized separation and simultaneous determination of seven steroid hormones in urine samples has been investigated. The isolation of analytes from biological samples was performed by liquid-liquid extraction (LLE with dichloromethane and compared to solid phase extraction (SPE with C18 and hydrophilic-lipophilic balance (HLB columns. To separate all the analytes a micellar electrokinetic capillary chromatography (MECK technique was employed. For full separation of all the analytes a running buffer (pH 9.2, composed of 10 mM sodium tetraborate decahydrate (borax, 50 mM sodium dodecyl sulfate (SDS, and 10% methanol was selected. The methodology developed in this work for the determination of steroid hormones meets all the requirements of analytical methods. The applicability of the method has been confirmed for the analysis of urine samples collected from volunteers—both men and women (students, amateur bodybuilders, using and not applying steroid doping. The data obtained during this work can be successfully used for further research on the determination of steroid hormones in urine samples.

  15. Diurnal and twenty-four hour patterning of human diseases: acute and chronic common and uncommon medical conditions.

    Science.gov (United States)

    Smolensky, Michael H; Portaluppi, Francesco; Manfredini, Roberto; Hermida, Ramon C; Tiseo, Ruana; Sackett-Lundeen, Linda L; Haus, Erhard L

    2015-06-01

    The symptom intensity and mortality of human diseases, conditions, and syndromes exhibit diurnal or 24 h patterning, e.g., skin: atopic dermatitis, urticaria, psoriasis, and palmar hyperhidrosis; gastrointestinal: esophageal reflux, peptic ulcer (including perforation and hemorrhage), cyclic vomiting syndrome, biliary colic, hepatic variceal hemorrhage, and proctalgia fugax; infection: susceptibility, fever, and mortality; neural: frontal, parietal, temporal, and occipital lobe seizures, Parkinson's and Alzheimer's disease, hereditary progressive dystonia, and pain (cancer, post-surgical, diabetic neuropathic and foot ulcer, tooth caries, burning mouth and temporomandibular syndromes, fibromyalgia, sciatica, intervertebral vacuum phenomenon, multiple sclerosis muscle spasm, and migraine, tension, cluster, hypnic, and paroxysmal hemicranial headache); renal: colic and nocturnal enuresis and polyuria; ocular: bulbar conjunctival redness, keratoconjunctivitis sicca, intraocular pressure and anterior ischemic optic neuropathy, and recurrent corneal erosion syndrome; psychiatric/behavioral: major and seasonal affective depressive disorders, bipolar disorder, parasuicide and suicide, dementia-associated agitation, and addictive alcohol, tobacco, and heroin cravings and withdrawal phenomena; plus autoimmune and musculoskeletal: rheumatoid arthritis, osteoarthritis, axial spondylarthritis, gout, Sjögren's syndrome, and systemic lupus erythematosus. Knowledge of these and other 24 h patterns of human pathophysiology informs research of their underlying circadian and other endogenous mechanisms, external temporal triggers, and more effective patient care entailing clinical chronopreventive and chronotherapeutic strategies.

  16. Twenty-four hour predictions of the solar wind speed peaks by the probability distribution function model

    Science.gov (United States)

    Bussy-Virat, C. D.; Ridley, A. J.

    2016-10-01

    Abrupt transitions from slow to fast solar wind represent a concern for the space weather forecasting community. They may cause geomagnetic storms that can eventually affect systems in orbit and on the ground. Therefore, the probability distribution function (PDF) model was improved to predict enhancements in the solar wind speed. New probability distribution functions allow for the prediction of the peak amplitude and the time to the peak while providing an interval of uncertainty on the prediction. It was found that 60% of the positive predictions were correct, while 91% of the negative predictions were correct, and 20% to 33% of the peaks in the speed were found by the model. This represents a considerable improvement upon the first version of the PDF model. A direct comparison with the Wang-Sheeley-Arge model shows that the PDF model is quite similar, except that it leads to fewer false positive predictions and misses fewer events, especially when the peak reaches very high speeds.

  17. Diurnal and twenty-four hour patterning of human diseases: cardiac, vascular, and respiratory diseases, conditions, and syndromes.

    Science.gov (United States)

    Smolensky, Michael H; Portaluppi, Francesco; Manfredini, Roberto; Hermida, Ramon C; Tiseo, Ruana; Sackett-Lundeen, Linda L; Haus, Erhard L

    2015-06-01

    Various medical conditions, disorders, and syndromes exhibit predictable-in-time diurnal and 24 h patterning in the signs, symptoms, and grave nonfatal and fatal events, e.g., respiratory ones of viral and allergic rhinorrhea, reversible (asthma) and non-reversible (bronchitis and emphysema) chronic obstructive pulmonary disease, cystic fibrosis, high altitude pulmonary edema, and decompression sickness; cardiac ones of atrial premature beats and tachycardia, paroxysmal atrial fibrillation, 3rd degree atrial-ventricular block, paroxysmal supraventricular tachycardia, ventricular premature beats, ventricular tachyarrhythmia, symptomatic and non-symptomatic angina pectoris, Prinzmetal vasospastic variant angina, acute (non-fatal and fatal) incidents of myocardial infarction, sudden cardiac arrest, in-bed sudden death syndrome of type-1 diabetes, acute cardiogenic pulmonary edema, and heart failure; vascular and circulatory system ones of hypertension, acute orthostatic postprandial, micturition, and defecation hypotension/syncope, intermittent claudication, venous insufficiency, standing occupation leg edema, arterial and venous branch occlusion of the eye, menopausal hot flash, sickle cell syndrome, abdominal, aortic, and thoracic dissections, pulmonary thromboembolism, and deep venous thrombosis, and cerebrovascular transient ischemic attack and hemorrhagic and ischemic stroke. Knowledge of these temporal patterns not only helps guide patient care but research of their underlying endogenous mechanisms, i.e., circadian and others, and external triggers plus informs the development and application of effective chronopreventive and chronotherapeutic strategies.

  18. The Twenty-four Hour Workday: Proceedings of a Symposium on Variations in Work-Sleep Schedules

    Science.gov (United States)

    1980-10-01

    Md. Tray.: 1971, _j 393-395. .ndlauer,P., Carpentier,J., & Cazamian,P. (Eds.). Ergonomie du travail de nuit et des horaires alternants. Education...and between subjects and suggest that Gaillard’s conclusion may not -be true. 743 REM 0) 2 {3 i4 40[ REM E 0L ɘ U 730-Delta Hour !Igure :2. Comuter

  19. Prevalence of type 1 brugada electrocardiographic pattern evaluated by twelve-lead twenty-four-hour holter monitoring.

    Science.gov (United States)

    Cerrato, Natascia; Giustetto, Carla; Gribaudo, Elena; Richiardi, Elena; Barbonaglia, Lorella; Scrocco, Chiara; Zema, Domenica; Gaita, Fiorenzo

    2015-01-01

    Patients with drug-induced type 1 Brugada electrocardiograms (BrECGs) are considered to have good prognosis. Spontaneous type 1 is, instead, considered a risk factor; however, it is probably underestimated because of the BrECG fluctuations. The aim of this study was to analyze, in a large population of patients with Br, the real prevalence of type 1 BrECG using 12-lead 24-hour Holter monitoring (12L-Holter) and its correlation with the time of the day. We recorded 303 12L-Holter in 251 patients. Seventy-five (30%) patients exhibited spontaneous type 1 BrECG at 12-lead ECG (group 1) and 176 (70%) had only drug-induced type 1 (group 2). Type 1 BrECG was defined as "persistent" (>85% of the recording), "intermittent" (Holter, 57% intermittent type 1%, and 31% never had type 1; in group 2, none had persistent type 1, 20% had intermittent type 1%, and 80% never showed type 1. To evaluate the circadian fluctuations of BrECG, 4 periods in the day were considered. Type 1 BrECG was more frequent between 12-noon and 6 p.m. (52%, p Holter than with conventional follow-up with periodic ECGs and this has important implications in the risk stratification. 12L-Holter recording might avoid 20% of the pharmacological challenges with sodium channel blockers, which are not without risks, and should thus be considered as the first screening test, particularly in children or in presence of borderline diagnostic basal ECG.

  20. Twenty-four hours or 10 days? A prospective randomised controlled trial in children comparing head bandages following pinnaplasty.

    Science.gov (United States)

    Ramkumar, S; Narayanan, V; Laing, J H E

    2006-01-01

    The perceived benefits of bandaging for 10 days following pinnaplasty have been questioned by previous studies. The problems arising from these dressings are many [Powell BWEM. The value of head dressings in the postoperative management of the prominent ear. Br J Plast Surg 1989;42:692-4. Bartley J. How long should ears be bandaged after otoplasty? J Laryngol Otol 1998;112:531-2. Wong MC, Sylaidis P. Head dressings for pinnaplasty: a tradition not supported by evidence. Br J Plast Surg 2001;54:81-2], including their slippage [Powell BWEM. The value of head dressings in the postoperative management of the prominent ear. Br J Plast Surg 1989;42:692-4. Bradbury ET, Hewison J, Timmons MJ. Psychological and social outcome of prominent ear correction in children. Br J Plast Surg 1992;45:97-100. Jeffery SLA. Complications following correction of prominent ears: an audit review of 122 cases. Br J Plast Surg 1999;52:588-90]. Eighty children were recruited into a prospective randomised controlled trial comparing the use of a head bandage for only 24 h with a standard practise of a 10-day head bandage. A preoperative measurement of the lateral ear projection (LEP) was made. The outcome measures recorded during the two planned postoperative visits at 10 days (visit 1) and 2 months (visit 2) were: patient satisfaction score, LEP, complications and any unscheduled hospital visits associated with the surgery. There was no significant difference in LEP and patient satisfaction between the two groups at both the scheduled postoperative visits. Differences between the groups in the number of unscheduled visits (p=0.21) did not reach statistical significance. The findings indicate that it is safe and effective to use head bandage for only 24 h following surgical correction of prominent ears. This study shows no benefit from the application of a formal head bandage for any longer than 1 day.

  1. Twenty-Four-Hour Urinary Aldosterone Predicts Inappropriate Left Ventricular Mass Index in Patients with Primary Aldosteronism

    Directory of Open Access Journals (Sweden)

    Chi-Sheng Hung

    2013-01-01

    Full Text Available Objective. Primary aldosteronism (PA is associated with inappropriate left ventricular hypertrophy (LVH in relation to a given gender and body size. There is no ideal parameter to predict the presence of LVH or inappropriate LVH in patients with PA. We investigate the performance of 24-hour urinary aldosterone level, plasma renin activity and aldosterone-to-renin ratio on this task. Methods. We performed echocardiography in 106 patients with PA and 31 subjects with essential hypertension (EH in a tertiary teaching hospital. Plasma renin activity, aldosterone concentration, and 24-hour urinary aldosterone level were measured. Results. Only 24-hour urinary aldosterone was correlated with left ventricular mass index (LVMI and excess LVMI among these parameters. The multivariate analysis revealed the urinary aldosterone level as an independent predictor for LVMI and excess LVMI. Analyzing the ability of urinary aldosterone, plasma aldosterone concentration, and plasma aldosterone-to-renin ratio to identify the presence of LVH (ROC AUC = 0.701, 0.568, 0.656, resp. and the presence of inappropriate LV mass index (defined as measured LVMI in predicting LVMI ratio >135% (ROC area under curve = 0.61, 0.43, 0.493, resp. revealed the better performance of 24-hour urinary aldosterone. Conclusions. In conclusion, 24-hour urinary aldosterone level performed better to predict the presence of LVH and inappropriate LVMI in patients with PA.

  2. Twenty-four hours hypothermia has temporary efficacy in reducing brain infarction and inflammation in aged rats

    DEFF Research Database (Denmark)

    Sandu, Raluca Elena; Buga, Ana Maria; Balseanu, Adrian Tudor

    2016-01-01

    inflammation and infarct size. However, after 1 week, the infarct size became even larger than in controls and after 2 weeks there was no beneficial effect on regenerative processes such as neurogenesis. Behaviorally, hypothermia also had a limited beneficial effect. Finally, after hydrogen sulfide...

  3. Twenty-four-hour exposure to altered blood flow modifies endothelial Ca2+-activated K+ channels in rat mesenteric arteries

    DEFF Research Database (Denmark)

    Hilgers, Rob H P; Janssen, Ger M J; Fazzi, Gregorio E

    2010-01-01

    ,5,12,16]tetraazacyclotricosine-5,13-diium dibromide (UCL 1684; inhibitor of SK3) or 1-[(2-chlorophenyl)diphenylmethyl]-1H-pyrazole (TRAM-34; inhibitor of IK1). In LF arteries, endothelium-dependent relaxation was markedly reduced, due to a reduction in the endothelium-derived hyperpolarizing factor (EDHF) response. In HF...

  4. Liquid chromatographic determination of quinolones in water and human urine samples after microextraction by packed sorbent.

    Science.gov (United States)

    Rani, Susheela; Kumar, Ashwini; Malik, Ashok Kumar; Singh, Baldev

    2012-01-01

    A method for the simultaneous determination of quinolones in water and urine samples by microextraction in a sorbent-packed syringe (MEPS) with LC is described. MEPS is a new miniaturized SPE technique that can be used with chromatographic instruments without any modifications. In MEPS, approximately 1 mg of the solid packing material is inserted into a syringe (100-250 microL) as a plug. Sample preparation takes place on the packed bed. The new method is promising, easy to use, economical, and rapid. The determination of quinolones in groundwater and urine was performed using MEPS as a sample preparation method with LC-UV determination. Four quinolone antibiotics--enrofloxacin, enoxacin, danofloxacin, and nalidixic acid--in groundwater and urine samples were used as analytes. The extraction recovery was found to be between 64.9 and 98.9%. The results showed high correlation coefficients (R2 > 0.992) for all of the analytes within the calibration range. The LOQ was between 0.091 and 0.315 ng/mL.

  5. Controversies in using urine samples for prostate cancer detection: PSA and PCA3 expression analysis

    Directory of Open Access Journals (Sweden)

    S. Fontenete

    2011-12-01

    Full Text Available PURPOSE: Prostate cancer (PCa is one of the most commonly diagnosed malignancies in the world. Although PSA utilization as a serum marker has improved prostate cancer detection it still presents some limitations, mainly regarding its specificity. The expression of this marker, along with the detection of PCA3 mRNA in urine samples, has been suggested as a new approach for PCa detection. The goal of this work was to evaluate the efficacy of the urinary detection of PCA3 mRNA and PSA mRNA without performing the somewhat embarrassing prostate massage. It was also intended to optimize and implement a methodological protocol for this kind of sampling. MATERIALS AND METHODS: Urine samples from 57 patients with suspected prostate disease were collected, without undergoing prostate massage. Increased serum PSA levels were confirmed by medical records review. RNA was extracted by different methods and a preamplification step was included in order to improve gene detection by Real-Time PCR. RESULTS: An increase in RNA concentration with the use of TriPure Isolation Reagent. Despite this optimization, only 15.8% of the cases showed expression of PSA mRNA and only 3.8% of prostate cancer patients presented detectable levels of PCA3 mRNA. The use of a preamplification step revealed no improvement in the results obtained. CONCLUSION: This work confirms that prostate massage is important before urine collection for gene expression analysis. Since PSA and PCA3 are prostate specific, it is necessary to promote the passage of cells from prostate to urinary tract, in order to detect these genetic markers in urine samples.

  6. The impact of free or standardized lifestyle and urine sampling protocol on metabolome recognition accuracy.

    Science.gov (United States)

    Wallner-Liebmann, Sandra; Gralka, Ewa; Tenori, Leonardo; Konrad, Manuela; Hofmann, Peter; Dieber-Rotheneder, Martina; Turano, Paola; Luchinat, Claudio; Zatloukal, Kurt

    2015-01-01

    Urine contains a clear individual metabolic signature, although embedded within a large daily variability. Given the potential of metabolomics to monitor disease onset from deviations from the "healthy" metabolic state, we have evaluated the effectiveness of a standardized lifestyle in reducing the "metabolic" noise. Urine was collected from 24 (5 men and 19 women) healthy volunteers over a period of 10 days: phase I, days 1-7 in a real-life situation; phase II, days 8-10 in a standardized diet and day 10 plus exercise program. Data on dietary intake and physical activity have been analyzed by a nation-specific software and monitored by published protocols. Urine samples have been analyzed by (1)H NMR followed by multivariate statistics. The individual fingerprint emerged and consolidated with increasing the number of samples and reaches ~100 % cross-validated accuracy for about 40 samples. Diet standardization reduced both the intra-individual and the interindividual variability; the effect was due to a reduction in the dispersion of the concentration values of several metabolites. Under standardized diet, however, the individual phenotype was still clearly visible, indicating that the individual's signature was a strong feature of the metabolome. Consequently, cohort studies designed to investigate the relation of individual metabolic traits and nutrition require multiple samples from each participant even under highly standardized lifestyle conditions in order to exploit the analytical potential of metabolomics. We have established criteria to facilitate design of urine metabolomic studies aimed at monitoring the effects of drugs, lifestyle, dietary supplements, and for accurate determination of signatures of diseases.

  7. Molecularly Imprinted Composite Membranes for Selective Detection of 2-Deoxyadenosine in Urine Samples

    Directory of Open Access Journals (Sweden)

    Sonia Scorrano

    2015-06-01

    Full Text Available An important challenge for scientific research is the production of artificial systems able to mimic the recognition mechanisms occurring at the molecular level in living systems. A valid contribution in this direction resulted from the development of molecular imprinting. In this work, a novel molecularly imprinted polymer composite membrane (MIM was synthesized and employed for the selective detection in urine samples of 2-deoxyadenosine (2-dA, an important tumoral marker. By thermal polymerization, the 2-dA-MIM was cross-linked on the surface of a polyvinylidene-difluoride (PVDF membrane. By characterization techniques, the linking of the imprinted polymer on the surface of the membrane was found. Batch-wise guest binding experiments confirmed the absorption capacity of the synthesized membrane towards the template molecule. Subsequently, a time-course of 2-dA retention on membrane was performed and the best minimum time (30 min to bind the molecule was established. HPLC analysis was also performed to carry out a rapid detection of target molecule in urine sample with a recovery capacity of 85%. The experiments indicated that the MIM was highly selective and can be used for revealing the presence of 2-dA in urine samples.

  8. Analysis of Fluconazole in Human Urine Sample by High Performance Liquid Chromatography Method

    Science.gov (United States)

    Hermawan, D.; Ali, N. A. Md; Ibrahim, W. A. Wan; Sanagi, M. M.

    2013-04-01

    A method for determination of fluconazole, antifungal drug in human urine by using reversed-phased high performance liquid chromatography (RP-HPLC) with ultraviolet (UV) detector was developed. Optimization HPLC conditions were carried out by changing the flow rate and composition of mobile phase. The optimum separation conditions at a flow rate 0.85 mL/min with a composition of mobile phase containing methanol:water (70:30, v/v) with UV detection at a wavelength 254 nm was able to analyze fluconazole within 3 min. The excellent linearity was obtained in the range of concentration 1 to 10 μg/mL with r2 = 0.998. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.39 μg/mL and 1.28 μg/mL, respectively. Solid phase extraction (SPE) method using octadecylsilane (C18) as a sorbent was used to clean-up and pre-concentrated of the urine sample prior to HPLC analysis. The average recoveries of fluconazole in spiked urine sample was 72.4% with RSD of 3.21% (n=3).

  9. [The detection of amphetamines in urine samples using immunochromatographic test strips].

    Science.gov (United States)

    Shanin, I A; Khan, O Iu; Petukhov, A E; Smirnov, A V; Eremin, S A

    2012-01-01

    This study has demonstrated the possibility of using immunochromatographic test strips for the reliable qualitative detection of amphetamine and methamphetamine in the urine samples at a cut-off level of 300 ng/ml. The test strips obtained from different manufactures are shown to be slightly different in terms of specificity as appears from the frequency of cross-reactions with various pharmaceutical products and narcotic drugs. Also, the use of the immunochromatographic strips makes it possible to determine amphetamine in a range of concentrations from 100 to 1000 ng/ml by measuring the intensity of test-line colour with the help of a TotalLab TL120 programmer and special scanning programs. The analysis for amphetamine using the NrcoStop (Osiris S) immunochromatographic strips failed to confirm the presence of this substance in the urine samples from the subjects who had drunk 0.5 l of energy drinks, such as Adrenaline RUSH, Red Bull, and Burn. It means that the presence of amphetamine in the urine should not be attributed to the consumption of such drinks.

  10. [Isolated yeast species in urine samples in a Spanish regional hospital].

    Science.gov (United States)

    Heras-Cañas, Victor; Ros, Luis; Sorlózano, Antonio; Gutiérrez-Soto, Blanca; Navarro-Marí, José María; Gutiérrez-Fernández, José

    2015-01-01

    Candiduria detection in hospitalized or immunocompromised patients is of great clinical significance. The aim of our study was to describe the isolation frequency of significant species of yeasts in urine samples processed in our hospital during the period 2010- 2013, and to analyze their susceptibility to commonly used antifungal agents. Species identification was performed by seeding on a chromogenic medium, the filamentation test and automated systems (ASM Vitek and MALDI Biotyper), while susceptibility was determined using the ASM Vitek system. Of the 632 yeast isolates in urine, 371 were Candida albicans species and 261 non-C. albicans Candida spp. The species with the highest number of resistant isolates were Candida glabrata and Candida krusei. Based on the results obtained, we believe that species identification and the susceptibility study should be current practice in the laboratories when species other than C. albicans are isolated.

  11. Comparison of uncertainties related to standardization of urine samples with volume and creatinine concentration

    DEFF Research Database (Denmark)

    Garde, Anne Helene; Hansen, Ase Marie; Kristiansen, Jesper

    2004-01-01

    When measuring biomarkers in urine, volume (and time) or concentration of creatinine are both accepted methods of standardization for diuresis. Both types of standardization contribute uncertainty to the final result. The aim of the present paper was to compare the uncertainty introduced when using...... the two types of standardization on 24 h samples from healthy individuals. Estimates of uncertainties were based on results from the literature supplemented with data from our own studies. Only the difference in uncertainty related to the two standardization methods was evaluated. It was found...... increase in convenience for the participants, when collecting small volumes rather than complete 24 h samples....

  12. Reliable Quantification of the Potential for Equations Based on Spot Urine Samples to Estimate Population Salt Intake: Protocol for a Systematic Review and Meta-Analysis

    OpenAIRE

    Huang, Liping; Crino, Michelle; Wu, Jason HY; Woodward, Mark; Land, Mary-Anne; McLean, Rachael; Webster, Jacqui; Enkhtungalag, Batsaikhan; Nowson, Caryl A; Elliott, Paul; Cogswell, Mary; Toft, Ulla; MILL, Jose G.; Furlanetto,Tania W.; Ilich, Jasminka Z.

    2016-01-01

    Background Methods based on spot urine samples (a single sample at one time-point) have been identified as a possible alternative approach to 24-hour urine samples for determining mean population salt intake. Objective The aim of this study is to identify a reliable method for estimating mean population salt intake from spot urine samples. This will be done by comparing the performance of existing equations against one other and against estimates derived from 24-hour urine samples. The effect...

  13. Arsenic speciation in clinical samples: urine analysis using fast micro-liquid chromatography ICP-MS.

    Science.gov (United States)

    Morton, Jackie; Leese, Elizabeth

    2011-02-01

    Arsenic speciation is a subject that is developing all the time both from improvements in analytical techniques and from increases in toxicological understanding. Despite speciation methods being widely developed, arsenic speciation is not routinely offered as an analysis in clinical laboratory. The work in this paper describes a simple routine method for arsenic speciation that could be easily implemented in clinical laboratories. The method described, a new, fast analytical method for arsenic speciation, is reported using micro-liquid chromatography hyphenated to an inductively coupled plasma mass spectrometer (μLC-ICP-MS). The method uses a low-pressure delivery six-port valve with a 5 cm anion exchange column, which allows a fully resolved separation of five arsenic species (arsenobetaine [AB], arsenite [As(3+)], arsenate [As(5+)], mono-methylarsonic acid [MMA(5+)] and dimethylarsinic acid [DMA(5+)]) in urine in just 6 min. This fast analytical method offers an arsenic speciation method that is feasible for a laboratory that does not have the capability for a dedicated arsenic speciation LC-ICP-MS instrument. The micro-LC system is small, easy to install and is fully integrated with the ICP-MS software. The results reported here are from urine samples from 65 workers in a semiconductor work providing a sample for their routine biological monitoring to assess workplace exposure. Control samples from 20 unexposed people were also determined. Results show that the semiconductor workers exhibit very low levels of arsenic in their urine samples, similar to the levels in the controls, and thus are not significantly exposed to arsenic. Care must be taken when interpreting urinary arsenic species results because it is not always possible to differentiate between dietary and other external sources of exposure.

  14. Validity of a portable urine refractometer: the effects of sample freezing.

    Science.gov (United States)

    Sparks, S Andy; Close, Graeme L

    2013-01-01

    The use of portable urine osmometers is widespread, but no studies have assessed the validity of this measurement technique. Furthermore, it is unclear what effect freezing has on osmolality. One-hundred participants of mean (±SD) age 25.1 ± 7.6 years, height 1.77 ± 0.1 m and weight 77.1 ± 10.8 kg provided single urine samples that were analysed using freeze point depression (FPD) and refractometry (RI). Samples were then frozen at -80°C (n = 81) and thawed prior to re-analysis. Differences between methods and freezing were determined using Wilcoxon's signed rank test. Relationships between measurements were assessed using intraclass correlation coefficients (ICC) and typical error of estimate (TE). Osmolality was lower (P = 0.001) using RI (634.2 ± 339.8 mOsm · kgH2O(-1)) compared with FPD (656.7 ± 334.1 mOsm · kgH2O(-1)) but the TE was trivial (0.17). Freezing significantly reduced mean osmolality using FPD (656.7 ± 341.1 to 606.5 ± 333.4 mOsm · kgH2O(-1); P < 0.001), but samples were still highly related following freezing (ICC, r = 0.979, P < 0.001, CI = 0.993-0.997; TE = 0.15; and r=0.995, P < 0.001, CI = 0.967-0.986; TE = 0.07 for RI and FPD respectively). Despite mean differences between methods and as a result of freezing, such differences are physiologically trivial. Therefore, the use of RI appears to be a valid measurement tool to determine urine osmolality.

  15. Loop Mediated Isothermal Amplification for Detection of Trypanosoma brucei gambiense in Urine and Saliva Samples in Nonhuman Primate Model

    Directory of Open Access Journals (Sweden)

    Maina Ngotho

    2015-01-01

    Full Text Available Human African trypanosomiasis (HAT is a vector-borne parasitic zoonotic disease. The disease caused by Trypanosoma brucei gambiense is the most prevalent in Africa. Early diagnosis is hampered by lack of sensitive diagnostic techniques. This study explored the potential of loop mediated isothermal amplification (LAMP and polymerase chain reaction (PCR in the detection of T. b. gambiense infection in a vervet monkey HAT model. Six vervet monkeys were experimentally infected with T. b. gambiense IL3253 and monitored for 180 days after infection. Parasitaemia was scored daily. Blood, cerebrospinal fluid (CSF, saliva, and urine samples were collected weekly. PCR and LAMP were performed on serum, CSF, saliva, and urine samples. The detection by LAMP was significantly higher than that of parasitological methods and PCR in all the samples. The performance of LAMP varied between the samples and was better in serum followed by saliva and then urine samples. In the saliva samples, LAMP had 100% detection between 21 and 77 dpi, whereas in urine the detection it was slightly lower, but there was over 80% detection between 28 and 91 dpi. However, LAMP could not detect trypanosomes in either saliva or urine after 140 and 126 dpi, respectively. The findings of this study emphasize the importance of LAMP in diagnosis of HAT using saliva and urine samples.

  16. Loop Mediated Isothermal Amplification for Detection of Trypanosoma brucei gambiense in Urine and Saliva Samples in Nonhuman Primate Model.

    Science.gov (United States)

    Ngotho, Maina; Kagira, John Maina; Gachie, Beatrice Muthoni; Karanja, Simon Muturi; Waema, Maxwell Wambua; Maranga, Dawn Nyawira; Maina, Naomi Wangari

    2015-01-01

    Human African trypanosomiasis (HAT) is a vector-borne parasitic zoonotic disease. The disease caused by Trypanosoma brucei gambiense is the most prevalent in Africa. Early diagnosis is hampered by lack of sensitive diagnostic techniques. This study explored the potential of loop mediated isothermal amplification (LAMP) and polymerase chain reaction (PCR) in the detection of T. b. gambiense infection in a vervet monkey HAT model. Six vervet monkeys were experimentally infected with T. b. gambiense IL3253 and monitored for 180 days after infection. Parasitaemia was scored daily. Blood, cerebrospinal fluid (CSF), saliva, and urine samples were collected weekly. PCR and LAMP were performed on serum, CSF, saliva, and urine samples. The detection by LAMP was significantly higher than that of parasitological methods and PCR in all the samples. The performance of LAMP varied between the samples and was better in serum followed by saliva and then urine samples. In the saliva samples, LAMP had 100% detection between 21 and 77 dpi, whereas in urine the detection it was slightly lower, but there was over 80% detection between 28 and 91 dpi. However, LAMP could not detect trypanosomes in either saliva or urine after 140 and 126 dpi, respectively. The findings of this study emphasize the importance of LAMP in diagnosis of HAT using saliva and urine samples.

  17. Analysis of epinephrine, norepinephrine, and dopamine in urine samples of hospital patients by micellar liquid chromatography.

    Science.gov (United States)

    García Ferrer, Daniel; García García, Aurelio; Peris-Vicente, Juan; Gimeno-Adelantado, José Vicente; Esteve-Romero, Josep

    2015-12-01

    An analytical method based on micellar liquid chromatography was developed to determine the concentration of three catecholamines (epinephrine, norepinephrine, and dopamine) in urine. The detection of these compounds in urine can be useful to diagnose several diseases, related to stress and sympathoadrenal system dysfunction, using a non-invasive collection procedure. The sample pretreatment was a simple dilution in a micellar solution, filtration, and direct injection, thus avoiding time-consuming and tedious extraction steps. Therefore, there is no need to use an internal standard. The three catecholamines were eluted using a C18 column and a mobile phase of 0.055 M sodium dodecyl sulfate-1.5% methanol buffered at pH 3.8 running at 1.5 mL/min under isocratic mode in less than 25 min. The detection was performed by amperometry applying a constant potential of +0.5 V. The procedure was validated following the guidelines of the European Medicines Agency in terms of the following: calibration range (0.09-5 μg/mL), linearity (r(2) > 0.9995), limit of detection (0.02 μg/mL), within- and between-run accuracy (-6.5 to +8.4%) and precision (<10.2%), dilution integrity, matrix effect, robustness (<8.4), and stability. The obtained values were below those required by the guide. The method was rapid, easy-to-handle, eco-friendly, and safe and provides reliable quantitative data, and is thus useful for routine analysis. The procedure was applied to the analysis of epinephrine, norepinephrine, and dopamine in urine samples from patients of a local hospital.

  18. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  19. Multisite Direct Determination of the Potential for Environmental Contamination of Urine Samples Used for Diagnosis of Sexually Transmitted Infections

    Science.gov (United States)

    Andersson, Patiyan; Tong, Steven Y. C.; Lilliebridge, Rachael A.; Brenner, Nicole C.; Martin, Louise M.; Spencer, Emma; Delima, Jennifer; Singh, Gurmeet; McCann, Frances; Hudson, Carolyn; Johns, Tracy; Giffard, Philip M.

    2014-01-01

    Background The detection of a sexually transmitted infection (STI) agent in a urine specimen from a young child is regarded as an indicator of sexual contact. False positives may conceivably arise from the transfer of environmental contaminants in clinic toilet or bathroom facilities into urine specimens. Methods The potential for contamination of urine specimens with environmental STI nucleic acid was tested empirically in the male and female toilets or bathrooms at 10 Northern Territory (Australia) clinics, on 7 separate occasions at each. At each of the 140 experiments, environmental contamination with Chlamydia trachomatis, Neisseria gonorrhoeae, and Trichomonas vaginalis nucleic acid contamination was determined by swabbing 10 locations, and urine collection was simulated 5 times, using a (1) synthetic urine surrogate and (2) a standardized finger contamination procedure. Results The most contaminated toilets and bathrooms were in remote Indigenous communities. No contamination was found in the Northern Territory Government Sexual Assault Referral Centre clinics, and intermediate levels of contamination were found in sexual health clinics and in clinics in regional urban centres. The frequency of surrogate urine sample contamination was low but non-zero. For example, 4 of 558 of the urine surrogate specimens from remote clinics were STI positive. Conclusions This is by far the largest study addressing the potential environmental contamination of urine samples with STI agents. Positive STI tests arising from environmental contamination of urine specimens cannot be ruled out. The results emphasize that urine specimens from young children taken for STI testing should be obtained by trained staff in clean environments, and duplicate specimens should be obtained if possible. PMID:25349693

  20. Determination of piroxicam in pharmaceutical formulations and urine samples using europium-sensitized luminescence

    Energy Technology Data Exchange (ETDEWEB)

    Al-Kindy, Salma M.Z. [Department of Chemistry, College of Science, P.O. Box 36, Al-Khod 123, Sultan Qaboos University (Oman)], E-mail: alkindy@squ.edu.om; Suliman, Fakhr Eldin O.; Al-Wishahi, Aisha A.; Al-Lawati, Haidar A.J.; Aoudia, Muhammed [Department of Chemistry, College of Science, P.O. Box 36, Al-Khod 123, Sultan Qaboos University (Oman)

    2007-12-15

    A simple, selective and sensitive luminescence method for the assay of piroxicam (PX) in aqueous solution is developed. The method is based on the luminescence sensitization of europium (Eu{sup 3+}) by formation of ternary complex with PX in the presence of TOPO and Tween-80 as surfactant. The signal for Eu-PX-TOPO is monitored at {lambda}{sub ex}=359 nm and {lambda}{sub em}=615 nm. Optimum conditions for the formation of the complex in sequential injection analysis (SIA) were 0.01 M Tris buffer, pH 7.5, TOPO 5.0x10{sup -5} M, Tween-80 0.15% and 1.5 mM of Eu{sup 3+}, which allows the determination of 100-1000 ppb of PX with limit of detection (LOD) of 29 ppb. The relative standard deviations of the method range between 0.5% and 3.9% indicating excellent reproducibility of the method. The proposed method was successfully applied for the assay of PX in pharmaceutical formulations and in urine samples. Average recoveries of 100.8{+-}1.7% was obtained in tablet, whereas a recovery of 97.5{+-}2.0% was obtained for the total PX (PX+hydoxy-PX) in urine sample.

  1. Detection of norfloxacin and monitoring its effect on caffeine catabolism in urine samples.

    Science.gov (United States)

    Agrawal, Bharati; Chandra, Pranjal; Goyal, Rajendra N; Shim, Yoon-Bo

    2013-09-15

    A multi-walled carbon nano tube (MWCNT) modified pyrolytic graphite (MPG) electrode is prepared and applied to detect norfloxacin (NFX) based on its electrochemical reduction. The experimental parameters affecting the NFX determination were optimized in terms of MWCNT amount, pH, reaction time, and square wave frequency. The dynamic range for the NFX analysis ranged between 1.2 and 1000µM with a detection limit of 40.6±3.3nM. The effect of NFX on the catabolism of caffeine has been studied by determining its concentration in the urine samples after the prolonged administration of NFX using the MPG electrode. The results show that the catabolism of caffeine is inhibited by ~65% after five days of NFX administration, consequently the caffeine concentration in the urine sample is increased, which is reflected in terms of ~2.5 times increase in the peak current of caffeine. The determinations of NFX and caffeine were selective and the method was successfully applied in biological fluids and pharmaceutical tablets for the test compound analysis. In future this method can be useful for the selective determination of NFX and studying its effect on caffeine catabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Diagnostic significance of atypical category in the voided urine samples: A retrospective study in a tertiary care center

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    Mokhtar Ghadeer

    2010-01-01

    Full Text Available Background: Voided urine samples continue to play an important role in the surveillance of urothelial malignancy and also as a screening mode for high risk patients. In some cases, it is difficult to reliably distinguish changes induced by inflammation, stone or other reactive condition from neoplasm, and these cases are categorized as atypical. The aim of our study is to evaluate the prevalence and the significance of atypical diagnosis in the voided urine samples and also to identify the cytomorphologic features that are seen more frequently in the atypical malignant urine samples. Materials and Methods: All voided urine cytology samples with a diagnosis of atypical urothelial cells, between the period of 2000 and 2009, were obtained from the cytology database. Only those cases with histologic follow-up were included in the study. The cytology and the histology slides were retrieved and reviewed. The following parameters were evaluated: cellularity, cell clusters, nuclear membrane irregularities, hyperchromasia and India-ink type nuclei, the presence of spindle cells and the cytoplasmic characteristics. Results: Out of 72 voided urine samples included in the study, 49 cases (68% had a positive histologic diagnosis of urothelial malignancy in the follow-up histology; of these (55% were high-grade urothelial carcinoma. Increased cellularity, papillary cell clusters, nuclear membrane irregularity, hyperchromasia and India-ink type nuclei were observed more frequently in the atypical malignant urine samples, while cytoplasmic vacuolization were seen more in the negative reactive urine samples. Conclusion: The atypical category diagnosis is associated with a significant proportion of urothelial carcinoma. It should be used by the pathologist to convey concern to the clinician in difficult cases that may require close follow-up.

  3. Validation of a Novel Collection Device for Non-Invasive Urine Sampling from Free-Ranging Animals.

    Directory of Open Access Journals (Sweden)

    Lisa Michelle Danish

    Full Text Available Recent advances in non-invasively collected samples have opened up new and exciting opportunities for wildlife research. Different types of samples, however, involve different limitations and certain physiological markers (e.g., C-peptide, oxytocin can only be reliably measured from urine. Common collection methods for urine to date work best for arboreal animals and large volumes of urine. Sufficient recovery of urine is thus still difficult for wildlife biologists, particularly for terrestrial and small bodied animals. We tested three collection devices (two commercially available saliva swabs, Salivette synthetic and cotton, and cotton First aid swabs against a control to permit the collection of small volumes of urine from the ground. We collected urine samples from captive and wild macaques, and humans, measured volume recovery, and analyzed concentrates of selected physiological markers (creatinine, C-peptide, and neopterin. The Salivette synthetic device was superior to the two alternative devices. Concentrations of creatinine, absolute C-peptide, C-peptide per creatinine, absolute neopterin, and neopterin per creatinine measured in samples collected with this device did not differ significantly from the control and were also strongly correlated to it. Fluid recovery was also best for this device. The least suitable device is the First aid collection device; we found that while absolute C-peptide and C-peptide per creatinine concentrations did not differ significantly from the control, creatinine concentrations were significantly lower than the control. In addition, these concentrations were either not or weakly correlated to the control. The Salivette cotton device provided intermediate results, although these concentrations were strongly correlated to the control. Salivette synthetic swabs seem to be useful devices for the collection of small amounts of urine from the ground destined for the assessment of physiological parameters. They

  4. Validation of a Novel Collection Device for Non-Invasive Urine Sampling from Free-Ranging Animals.

    Science.gov (United States)

    Danish, Lisa Michelle; Heistermann, Michael; Agil, Muhammad; Engelhardt, Antje

    2015-01-01

    Recent advances in non-invasively collected samples have opened up new and exciting opportunities for wildlife research. Different types of samples, however, involve different limitations and certain physiological markers (e.g., C-peptide, oxytocin) can only be reliably measured from urine. Common collection methods for urine to date work best for arboreal animals and large volumes of urine. Sufficient recovery of urine is thus still difficult for wildlife biologists, particularly for terrestrial and small bodied animals. We tested three collection devices (two commercially available saliva swabs, Salivette synthetic and cotton, and cotton First aid swabs) against a control to permit the collection of small volumes of urine from the ground. We collected urine samples from captive and wild macaques, and humans, measured volume recovery, and analyzed concentrates of selected physiological markers (creatinine, C-peptide, and neopterin). The Salivette synthetic device was superior to the two alternative devices. Concentrations of creatinine, absolute C-peptide, C-peptide per creatinine, absolute neopterin, and neopterin per creatinine measured in samples collected with this device did not differ significantly from the control and were also strongly correlated to it. Fluid recovery was also best for this device. The least suitable device is the First aid collection device; we found that while absolute C-peptide and C-peptide per creatinine concentrations did not differ significantly from the control, creatinine concentrations were significantly lower than the control. In addition, these concentrations were either not or weakly correlated to the control. The Salivette cotton device provided intermediate results, although these concentrations were strongly correlated to the control. Salivette synthetic swabs seem to be useful devices for the collection of small amounts of urine from the ground destined for the assessment of physiological parameters. They thus provide new

  5. Liquid Chromatographic Determination of Pioglitazone in Pharmaceuticals, Serum and Urine Samples

    Directory of Open Access Journals (Sweden)

    Shahnaz Perveen

    2011-12-01

    Full Text Available A rapid and reliable analytical method based on high-performance liquid chromatography (HPLC with UV detection (221nm has been developed for the determination of the anti-hyperglycemic agent Pioglitazone in pharmaceutical formulations and biological fluids (serum and urine after clean-up with solid-phase extraction. Chromatographic separation was achieved with a Chromolith® Performance RP-18e (100×4.6mm column using mobile phase composition of acetonitrile: mixed phosphate buffer (pH 2.5; 10mM (30:70, v/v with a flow rate of 2.0mL/min. The total run time was 2 min. under optimized conditions. The calibration curve was found to be linear in the range of 1-10 µg mL-1 with regression coefficient of 0.9996, and the lower limit of detection 72 ng/20µL injection. The method has been validated for the system suitability, linearity, precision and accuracy, limits of detection, specificity, stability and robustness. The %recovery of Pioglitazone in pharmaceutical formulations was found to be 104.7%. The assay has been applied successfully to the pharmaceutical Tablet samples and biological fluids (serum and urine of healthy volunteers.

  6. [Bacteria isolated from urine and renal tissue samples and their relation to renal histology].

    Science.gov (United States)

    Gökalp, A; Gültekin, E Y; Bakici, M Z; Ozdeşlik, B

    1988-01-01

    The bacteria from the urine and renal biopsy specimens of 40 patients undergoing renal surgery were isolated and their relations with renal histology investigated. The urine cultures were positive in 14 patients, the same organisms being isolated from the renal tissue in 7 cases. In 6 patients with negative urine cultures, bacteria were isolated from renal tissues. Of the 28 cases pathologically diagnosed as chronic pyelonephritis, bacteria were isolated from the renal tissue in 13 cases, the urine cultures being positive in only 11 cases. E. coli was the most commonly encountered bacteria in both the urine and renal tissues.

  7. Post mortem concentrations of endogenous gamma hydroxybutyric acid (GHB) and in vitro formation in stored blood and urine samples.

    Science.gov (United States)

    Busardò, Francesco Paolo; Bertol, Elisabetta; Vaiano, Fabio; Baglio, Giovanni; Montana, Angelo; Barbera, Nunziata; Zaami, Simona; Romano, Guido

    2014-10-01

    Gamma-hydroxybutyrate (GHB) is a central nervous system depressant, primarily used as a recreational drug of abuse with numerous names. It has also been involved in various instances of drug-facilitated sexual assault due to its potential incapacitating effects. The first aim of this paper is to measure the post-mortem concentration of endogenous GHB in whole blood and urine samples of 30 GHB free-users, who have been divided according to the post-mortem interval (PMI) in three groups (first group: 24-36h; second group: 37-72h; third group: 73-192h), trying to evaluate the role of PMI in affecting post mortem levels. Second, the Authors have evaluated the new formation of GHB in vitro in blood and urine samples of the three groups, which have been stored at -20°C, 4°C and 20°C over a period of one month. The concentrations were measured by GC-MS after liquid-liquid extraction according to the method validated and published by Elliot (For. Sci. Int., 2003). For urine samples, GHB concentrations were creatinine-normalized. In the first group the GHB mean concentration measured after autopsy was: 2.14mg/L (range 0.54-3.21mg/L) in blood and 3.90mg/g (range 0.60-4.81mg/g) in urine; in the second group it was: 5.13mg/L (range 1.11-9.60mg/L) in blood and 3.93mg/g (range 0.91-7.25mg/g) in urine; in the third group it was: 11.8mg/L (range 3.95-24.12mg/L) in blood and 9.83mg/g (range 3.67-21.90mg/g) in urine. The results obtained in blood and urine samples showed a statistically significant difference among groups (pGHB in blood and urine samples. Regarding the new formation of GHB in vitro both in blood and urine samples of the three groups, which have been stored at -20°C, 4°C and 20°C over a period of one month, although there was no significant increases of GHB levels throughout the period of investigation, the lowest increases were found both in blood and urine at -20°C, therefore we recommend the latter as optimal storage temperature.

  8. Capillary gas-liquid chromatography separation of phenethylamines in amphetamine-positive urine samples.

    Science.gov (United States)

    DePace, A; Verebey, K; elSohly, M

    1990-11-01

    Good gas chromatography (GC) separation of molecules is essential for clean gas chromatography/mass spectrometry (GC/MS) confirmation of compounds. The trifluoro derivatives of ephedrine (E) and methamphetamine (MA) coelute on dimethyl silicone capillary columns, such as DB-1, which are most commonly used by chromatographers. Methods are described to separate E and MA to aid GC/MS confirmations of methamphetamine, ephedrine, or both E and MA together, whichever may be present in Enzyme Immunoassay (EIA)-analyzed amphetamine-positive urine samples. The use of the heptafluoro derivatives of E and MA on a DB-1 column, or the trifluoro derivatives of E and MA on a DB-17 column, is suggested for good gas chromatographic separation.

  9. The examination of urine samples for pathogenic microbes by the luciferase assay for ATP. 1: The effect of the presence of fungi, fungal like bacteria and kidney cells in urine samples

    Science.gov (United States)

    Bush, V. N.

    1973-01-01

    A method for accurately determining urinary tract infections in man is introduced. The method is based on adenosine triphosphate (ATP) concentration in urine samples after removing nonbacterial ATP. Adenosine triphosphate concentration is measured from the bioluminescent reaction of luciferase when mixed with ATP. An examination was also made of the effectiveness of rupturing agents on monkey kidney cells Candia albicans, a Rhodotorula species, and a Streptomyces species in determining whether these cells could contribute ATP to the bacterial ATP value of a urine sample.

  10. Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gao, Lina; Liu, Junting; Wang, Chunyuan; Liu, Guojie; Niu, Xiaodong; Shu, Cuixia; Zhu, Juan

    2014-01-01

    A simple, sensitive and reliable gas chromatographic-mass spectrometric method (GC-MS) for quantifying paraquat concentration in biological samples has been developed, using ethyl paraquat as an internal standard. The method involved the procedures of sodium borohydride-nickel chloride (NaBH4-NiCl2) reduction and solid-phase microextraction (SPME) of the perhydrogenated products. GC-MS was used to identify and quantify the analytes in selected ion monitoring (SIM) mode. Under the optimal conditions, recoveries in plasma and urine samples were 94.00-99.85% and 95.00-100.34%, respectively. Excellent sample clean-up was observed and good linearities (r=0.9982 for plasma sample and 0.9987 for urine sample) were obtained in the range of 0.1-50μg/mL. The limits of detection (S/N=3) were 0.01μg/mL in plasma and urine samples. The intra-day precision was less than 8.43%, 4.19% (n=3), and inter-day precision was less than 10.90%, 10.49% (n=5) for plasma and urine samples, respectively. This method was successfully applied to the analysis of the biological samples collected from a victim who died as a result of ingestion of paraquat.

  11. Blood and urine samples as useful sources for the direct detection of tuberculosis by polymerase chain reaction.

    Science.gov (United States)

    Rebollo, María J; San Juan Garrido, Rafael; Folgueira, Dolores; Palenque, Elia; Díaz-Pedroche, C; Lumbreras, Carlos; Aguado, José M

    2006-10-01

    The aim of the study was to assess the utility of the polymerase chain reaction (PCR) assay in blood and urine for the diagnosis of tuberculosis (TB). We prospectively evaluated the usefulness of PCR performed in blood and urine samples from patients with proved or probable TB compared with a control group of patients. The PCR technique was performed using IS6110 primers. We included in the study 57 patients (43 with definite TB and 14 with probable TB) and 26 controls. Blood and urine samples were drawn at the time of microbiologic diagnosis and 3, 6, 9, and 12 months later. Cultures were positive in the early period (<1 month after treatment) in 11 of 57 patients (19%) with probable or definite TB, in comparison with 42% of patients (24/57) who yielded a positive PCR (P = 0.02). Urine samples increased the sensitivity of PCR determination in blood samples by 10%. The PCR in blood and/or urine was positive in 41% of patients with pulmonary TB, in 36% of patients with extrapulmonary TB, and in 50% of patients with disseminated TB. Mycobacterium tuberculosis was still detectable by PCR in 5 of 13 patients with cured TB after 1 or more months of antituberculous treatment. The PCR detection of M. tuberculosis in blood and urine samples is useful for the diagnosis of different clinical forms of TB, mostly in those patients in which sample extraction is difficult or requires aggressive techniques. The sensitivity of this technique could be improved studying more than 1 sample in each patient, even after initiating an antituberculous treatment.

  12. Genotyping of Leptospira directly in urine samples of cattle demonstrates a diversity of species and strains in Brazil.

    Science.gov (United States)

    Hamond, C; Pestana, C P; Medeiros, M A; Lilenbaum, W

    2016-01-01

    The aim of this study was to identify Leptospira in urine samples of cattle by direct sequencing of the secY gene. The validity of this approach was assessed using ten Leptospira strains obtained from cattle in Brazil and 77 DNA samples previously extracted from cattle urine, that were positive by PCR for the genus-specific lipL32 gene of Leptospira. Direct sequencing identified 24 (31·1%) interpretable secY sequences and these were identical to those obtained from direct DNA sequencing of the urine samples from which they were recovered. Phylogenetic analyses identified four species: L. interrogans, L. borgpetersenii, L. noguchii, and L. santarosai with the most prevalent genotypes being associated with L. borgpetersenii. While direct sequencing cannot, as yet, replace culturing of leptospires, it is a valid additional tool for epidemiological studies. An unexpected finding from this study was the genetic diversity of Leptospira infecting Brazilian cattle.

  13. Exploring the concurrent presence of hepatitis A virus genome in serum, stool, saliva, and urine samples of hepatitis A patients.

    Science.gov (United States)

    Joshi, Madhuri S; Bhalla, Shilpa; Kalrao, Vijay R; Dhongade, Ramchandra K; Chitambar, Shobha D

    2014-04-01

    The use of saliva and urine as an alternative to serum samples for detection of anti-hepatitis A virus (HAV) IgM antibodies has been documented. However, these samples remain underreported or unexplored for shedding of HAV. To address this issue, paired serum, stool, saliva, and urine samples collected from hepatitis A patients were screened by reverse transcription polymerase chain reaction for detection of HAV RNA. HAV RNA was detected in 67.6% (44/65), 52.3% (34/65), 8.7% (5/57), and 12.3% (8/65) of the serum, stool, saliva, and urine samples, respectively. Phylogenetic analysis of nucleotide sequences obtained for partial RNA polymerase region grouped HAV strains from all of the clinical samples of the study in subgenotype IIIA. Low frequency of HAV nucleic acid in saliva and urine samples indicates limited utility of these samples in genomic studies on HAV but suggests its potential for transmission and infection of hepatitis A.

  14. Associations between individual lower urinary tract symptoms and bacteriuria in random urine samples in women.

    Science.gov (United States)

    Sorrentino, Felice; Cartwright, Rufus; Digesu, G Alessandro; Tolton, Louise; Franklin, Larissa; Singh, Anand; Greco, Pantaleo; Khullar, Vik

    2015-06-01

    Previous studies have noted an association between a diagnosis of overactive bladder and bacteriuria, but little is understood about the relationship of bacteriuria to specific LUTS. We hypothesized that bacteriuria in women would be associated with increased self-reported symptom scores for a wide range of LUTS. Women were recruited from general gynecology and urogynecology outpatient clinics in a secondary care setting. Women completed the 12-item International Consultation on Incontinence Questionnaire for Female Lower Urinary Tract Symptoms and provided a clean-catch mid-stream specimen of urine for microscopy and culture. Women with acute urinary tract infection were excluded. Three statistical approaches (Mann-Whitney U-test, multivariable logistic regression, and receiver operating characteristic curves) were used to assess differences in symptom scores between women with and without bacteriuria. Two hundred forty-seven women were recruited, aged 22-82. Sixteen of 247 urine samples (6.5%) demonstrated significant bacteriuria, growing a different range of organisms. Women with significant bacteriuria were more likely to have nocturia (OR 3.56, 95% CI 1.19-10.6, P = 0.02), urgency (OR 6.66, 95% CI 1.47-30.06, P = 0.01), bladder pain (OR 2.82, 95% CI 1-7.92, P = 0.049), urgency incontinence (OR 2.92, 95% CI 1.02-8.36, P = 0.046), nocturnal enuresis (OR 4.21, 95% CI 1.32-13.41, P = 0.01). After adjustment for age, parity, symptomatic prolapse, menopausal status and history of mid-urethral sling urinary urgency, bladder pain, nocturia, and nocturnal enuresis remained significantly associated. Bacteriuria is associated with a range of LUTS including nocturia, urgency, and bladder pain supporting a role for bacterial colonization in the pathogenesis of OAB symptoms. © 2014 Wiley Periodicals, Inc.

  15. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    OpenAIRE

    Andrada,Daniel; Pinto,Frederico G.; Magalhães, Cristina Gonçalves; Nunes,Berta R.; Franco,Milton B.; Silva,José Bento Borba da

    2006-01-01

    The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cup...

  16. Parabens in 24 h urine samples of the German Environmental Specimen Bank from 1995 to 2012.

    Science.gov (United States)

    Moos, Rebecca K; Koch, Holger M; Angerer, Jürgen; Apel, Petra; Schröter-Kermani, Christa; Brüning, Thomas; Kolossa-Gehring, Marike

    2015-10-01

    Parabens are widely used as antimicrobial preservatives in personal care and consumer products, food and pharmaceuticals. Due to their ubiquity, humans are constantly exposed to these chemicals. We assessed exposure to nine parabens (methyl-, ethyl-, n- and iso-propyl-, n- and iso-butyl-, benzyl-, pentyl- and heptyl paraben) in the German population from 1995 to 2012 based on 660 24h urine samples from the German Environmental Specimen Bank (ESB) using on-line HPLC coupled to isotope dilution tandem mass spectrometry. The limit of quantification (LOQ) was 0.5 μg/L for all parabens. We detected methyl-, ethyl- and n-propyl paraben in 79-99% of samples, followed by n-butyl paraben in 40% of samples. We infrequently detected iso-butyl-, iso-propyl- and benzyl paraben in 24%, 4% and 1.4% of samples, respectively. Urinary concentrations were highest for methyl paraben (median 39.8 μg/L; 95th percentile 319 μg/L) followed by n-propyl paraben (4.8 μg/L; 95th percentile 74.0 μg/L) and ethyl paraben (2.1 μg/L; 95th percentile 39.1 μg/L). Women had significantly higher urinary levels for all parabens than men, except for benzyl paraben. Samples from the ESB revealed that over the investigation period of nearly 20 years urinary paraben levels remained surprisingly constant; only methyl paraben had a significant increase, for both men and women. We found strong correlations between methyl- and n-propyl paraben and between n- and iso-butyl paraben. These results indicate that parabens are used in combination and arise from common sources of exposure. Urinary excretion factors are needed to extrapolate from individual urinary concentrations to actual doses. Copyright © 2015 Elsevier GmbH. All rights reserved.

  17. Quantifying cobalt in doping control urine samples--a pilot study.

    Science.gov (United States)

    Krug, Oliver; Kutscher, Daniel; Piper, Thomas; Geyer, Hans; Schänzer, Wilhelm; Thevis, Mario

    2014-01-01

    Since first reports on the impact of metals such as manganese and cobalt on erythropoiesis were published in the late 1920s, cobaltous chloride became a viable though not widespread means for the treatment of anaemic conditions. Today, its use is de facto eliminated from clinical practice; however, its (mis)use in human as well as animal sport as an erythropoiesis-stimulating agent has been discussed frequently. In order to assess possible analytical options and to provide relevant information on the prevalence of cobalt use/misuse among athletes, urinary cobalt concentrations were determined by inductively coupled plasma-mass spectrometry (ICP-MS) from four groups of subjects. The cohorts consisted of (1) a reference population with specimens of 100 non-elite athletes (not being part of the doping control system), (2) a total of 96 doping control samples from endurance sport athletes, (3) elimination study urine samples collected from six individuals having ingested cobaltous chloride (500 µg/day) through dietary supplements, and (4) samples from people supplementing vitamin B12 (cobalamin) at 500 µg/day, accounting for approximately 22 µg of cobalt. The obtained results demonstrated that urinary cobalt concentrations of the reference population as well as the group of elite athletes were within normal ranges (0.1-2.2 ng/mL). A modest but significant difference between these two groups was observed (Wilcoxon rank sum test, p cobalt levels. The elimination study urine specimens yielded cobalt concentrations between 40 and 318 ng/mL during the first 6 h post-administration, and levels remained elevated (>22 ng/mL) up to 33 h. Oral supplementation of 500 µg of cobalamin did not result in urinary cobalt concentrations > 2 ng/mL. Based on these pilot study data it is concluded that measuring the urinary concentration of cobalt can provide information indicating the use of cobaltous chloride by athletes. Additional studies are however

  18. Urine versus brushed samples in human papillomavirus screening: study in both genders.

    NARCIS (Netherlands)

    Hauwers, K.W.M. d'; Depuydt, C.; Bogers, J.P.; Stalpaert, M.; Vereecken, A.; Wyndaele, J.J.; Tjalma, W.

    2007-01-01

    AIM: To investigate whether urine is a good medium for screening and whether there is a correlation between the amount of extracted DNA and human papillomavirus (HPV)-positivity. METHODS: In the present study, 30 first-voided urine (FVU) specimens and 20 urethroglandular swabs using cervex-brushes f

  19. Real-time detection of the chemokine CXCL12 in urine samples by surface plasmon resonance.

    Science.gov (United States)

    Vega, Beatriz; Calle, Ana; Sánchez, Alejandra; Lechuga, Laura M; Ortiz, Ana M; Armelles, Gaspar; Rodríguez-Frade, José Miguel; Mellado, Mario

    2013-05-15

    Surface plasmon resonance (SPR)-based biosensors are established tools for measuring biomolecular interactions between unlabeled analytes in real time, and are thus an ideal method to evaluate G protein-coupled receptor (GPCR) binding interactions. Using as a vehicle lentiviral particles bearing the chemokine receptor CXCR4 in its native plasma membrane context, SPR analysis can be performed using the particles as specific receptors to monitor the CXCR4 interaction with its ligand, CXCL12. The method shows linear correlation in the 5-40 nM range, with low intra- and inter-assay variation, a relative standard deviation <10%, chip-to-chip variation <12%, with stability of the sensor response for more than 150 measurements in the same chip over a four-week period. Our objective was to develop a method for rapid detection and quantification of analytes such as CXCL12 in biological samples, with no need for pretreatment. As a proof of concept, we tested for CXCL12 in urine samples from rheumatoid arthritis patients, who have elevated levels of this chemokine in plasma and synovial fluid. The biosensor method allowed sensitive, reproducible CXCL12 detection in the physiological range, suggesting its value for the diagnosis of autoimmune disorders.

  20. Comparing urine samples and cervical swabs for Chlamydia testing in a female population by means of Strand Displacement Assay (SDA

    Directory of Open Access Journals (Sweden)

    Wentzel-Larsen Tore

    2010-03-01

    Full Text Available Abstract Background There has been an increasing number of diagnosed cases of Chlamydia trachomatis in many countries, in particular among young people. The present study was based on a growing request to examine urine as a supplementary or primary specimen in screening for Chlamydia trachomatis in women, with the Becton Dickinson ProbeTec (BDPT Strand Displacement Assay (SDA. Urine samples may be particularly important in screening young people who are asymptomatic. Methods A total of 603 women aged 15 and older were enrolled from the Sexually Transmitted Infection (STI clinic at Haukeland University Hospital, Norway, in 2007. Only 31 women were older than 35 years. Cervical swabs and urine samples were tested with BDPT for all participants. In cases of discrepant test results from a given patient, both samples were retested by Cobas TaqManCT and a Polymerase Chain Reaction (PCR-method (in-house. Prevalence of C. trachomatis, sensitivity, and specificity were estimated by latent class analysis using all test results available. Bootstrap BC confidence intervals (10 000 computations were estimated for sensitivity and specificity, and their differences in cervix vs. urine tests. Results A total of 1809 specimens were collected from 603 patients. 80 women (13.4% were positive for C. trachomatis. Among these, BDPT identified 72 and 73 as positive in cervix and urine samples, respectively. Of the 523 C. trachomatis negative women, BDPT identified 519 as negative based on cervical swabs, and 514 based on urine samples. Sensitivity for cervical swabs and urine samples with the BDPT were 89.0% (95% CI 78.8, 98.6 and 90.2% (95% CI 78.1, 95.5, respectively. The corresponding values for specificity were 99.2% (95% CI 98.3, 100 and 98.3% (95% CI 96.4, 100. Conclusions This study indicates that urine specimens are adequate for screening high-risk groups for C. trachomatis by the SDA method (BDPT. Such an approach may facilitate early detection and treatment

  1. Calcium isolation from large-volume human urine samples for 41Ca analysis by accelerator mass spectrometry.

    Science.gov (United States)

    Miller, James J; Hui, Susanta K; Jackson, George S; Clark, Sara P; Einstein, Jane; Weaver, Connie M; Bhattacharyya, Maryka H

    2013-08-01

    Calcium oxalate precipitation is the first step in preparation of biological samples for (41)Ca analysis by accelerator mass spectrometry. A simplified protocol for large-volume human urine samples was characterized, with statistically significant increases in ion current and decreases in interference. This large-volume assay minimizes cost and effort and maximizes time after (41)Ca administration during which human samples, collected over a lifetime, provide (41)Ca:Ca ratios that are significantly above background.

  2. Calcium Isolation from Large-Volume Human Urine Samples for 41Ca Analysis by Accelerator Mass Spectrometry

    Science.gov (United States)

    Miller, James J; Hui, Susanta K; Jackson, George S; Clark, Sara P; Einstein, Jane; Weaver, Connie M; Bhattacharyya, Maryka H

    2013-01-01

    Calcium oxalate precipitation is the first step in preparation of biological samples for 41Ca analysis by accelerator mass spectrometry. A simplified protocol for large-volume human urine samples was characterized, with statistically significant increases in ion current and decreases in interference. This large-volume assay minimizes cost and effort and maximizes time after 41Ca administration during which human samples, collected over a lifetime, provide 41Ca:Ca ratios that are significantly above background. PMID:23672965

  3. Temporal variability of pyrethroid metabolite levels in bedtime, morning, and 24-h urine samples for 50 adults in North Carolina.

    Science.gov (United States)

    Morgan, Marsha K; Sobus, Jon R; Barr, Dana Boyd; Croghan, Carry W; Chen, Fu-Lin; Walker, Richard; Alston, Lillian; Andersen, Erik; Clifton, Matthew S

    2016-01-01

    Pyrethroid insecticides are widely used to control insects in both agricultural and residential settings worldwide. Few data are available on the temporal variability of pyrethroid metabolites in the urine of non-occupationally exposed adults. In this work, we describe the study design and sampling methodology for the Pilot Study to Estimate Human Exposures to Pyrethroids using an Exposure Reconstruction Approach (Ex-R study). Two major objectives were to quantify the concentrations of several pyrethroid metabolites in bedtime, first morning void (FMV), and 24-h urine samples as concentration (wet weight), specific-gravity (SG) corrected, creatinine (CR) corrected, and excretion rate values for 50 Ex-R adults over a six-week monitoring period and to determine if these correction approaches for urine dilution reduced the variability of the biomarker levels. The Ex-R study was conducted at the United States Environmental Protection Agency's Human Studies Facility in Chapel Hill, North Carolina USA and at participants' homes within a 40-mile radius of this facility. Recruitment of participants and field activities occurred between October 2009 and May 2011. Participants, ages 19-50 years old, provided daily food, activity, and pesticide-use diaries and collected their own urine samples (bedtime, FMV, and 24-h) during weeks 1, 2, and 6 of a six-week monitoring period. A total of 2503 urine samples were collected from the study participants. These samples were analyzed for the pyrethroid metabolites 3-phenoxybenzoic acid (3-PBA), cis/trans-3-(2,2-dichlorovinyl)-2,2-dimethyl-cyclopropane carboxylic acid (cis/trans-DCCA), and 2-methyl-3-phenylbenzoic acid (MPA) using high performance liquid chromatography/tandem mass spectrometry. Only 3-PBA was frequently detected (>50%) in the adult urine samples. Median urinary 3-PBA levels were 0.88 ng/mL, 0.96 ng/mL-SG, 1.04 ng/mg, and 1.04 ng/min for concentration, SG-corrected, CR-corrected, and excretion rate values, respectively

  4. Selenium speciation in human urine samples by LC- and CE-ICP-MS-separation and identification of selenosugars

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Bendahl, L.

    2004-01-01

    Human urine samples were analysed by a reversed-phase chromatographic system and an ion-pair chromatographic system. The chromatographic system, was connected to the ICP-MS either by a microconcentric nebulizer (MCN) in combination with a cyclonic spraychamber or by a modified direct injection...

  5. Direct Analysis of Amphetamine Stimulants in a Whole Urine Sample by Atmospheric Solids Analysis Probe Tandem Mass Spectrometry

    Science.gov (United States)

    Crevelin, Eduardo J.; Salami, Fernanda H.; Alves, Marcela N. R.; De Martinis, Bruno S.; Crotti, Antônio E. M.; Moraes, Luiz A. B.

    2016-05-01

    Amphetamine-type stimulants (ATS) are among illicit stimulant drugs that are most often used worldwide. A major challenge is to develop a fast and efficient methodology involving minimal sample preparation to analyze ATS in biological fluids. In this study, a urine pool solution containing amphetamine, methamphetamine, ephedrine, sibutramine, and fenfluramine at concentrations ranging from 0.5 pg/mL to 100 ng/mL was prepared and analyzed by atmospheric solids analysis probe tandem mass spectrometry (ASAP-MS/MS) and multiple reaction monitoring (MRM). A urine sample and saliva collected from a volunteer contributor (V1) were also analyzed. The limit of detection of the tested compounds ranged between 0.002 and 0.4 ng/mL in urine samples; the signal-to-noise ratio was 5. These results demonstrated that the ASAP-MS/MS methodology is applicable for the fast detection of ATS in urine samples with great sensitivity and specificity, without the need for cleanup, preconcentration, or chromatographic separation. Thus ASAP-MS/MS could potentially be used in clinical and forensic toxicology applications.

  6. Simultaneous kinetic spectrophotometric determination of norfloxacin and rifampicin in pharmaceutical formulation and human urine samples by use of chemometrics approaches

    Institute of Scientific and Technical Information of China (English)

    KOKOT; Serge

    2008-01-01

    A kinetic spectrophotometric method with aid of chemometrics is proposed for the simultaneous determination of norfloxacin and rifampicin in mixtures. The proposed method was applied for the simultaneous determination of these two compounds in pharmaceutical formulation and human urine samples,and the results obtained are similar to those obtained by high performance liquid chromatography.

  7. Silver nanoparticles enhanced flow injection chemiluminescence determination of gatifloxacin in pharmaceutical formulation and spiked urine sample

    Science.gov (United States)

    Wabaidur, Saikh mohammad; Alam, Seikh Mafiz; Alothman, Zeid A.; Mohsin, Kazi

    2015-06-01

    Silver nanoparticles have been utilized for the enhanced chemiluminogenic estimation of fluoroquinolone antibiotic gatifloxacin. It has been found that the weak chemiluminescence intensity produced from the reaction between calcein and KMnO4 can further be strengthened by the addition of silver nanoparticles in the presence of gatifloxacin. This phenomenon has been exploited to the quantitative determination of gatifloxacin. Under the optimum experimental conditions, the calibration curves are linear over the range of 8.9 × 10-9-4.0 × 10-6 M, while the limits of detections were found to be 2.6 × 10-9 M with correlation coefficient value (r2) 0.9999. The relative standard deviation calculated from six replicate measurements (1.0 × 10-4 M gatifloxacin) was 1.70%. The method was applied to pharmaceutical preparations and the results obtained were in reasonable agreement with the amount labeled on the formulations. The proposed method was also used for the determination of gatifloxacin in spiked urine samples with satisfactory results. No interference effects from some common excipients used in pharmaceutical preparations have been found.

  8. Determination of human albumin in serum and urine samples by constant-energy synchronous fluorescence method.

    Science.gov (United States)

    Madrakian, Tayyebeh; Bagheri, Habibollah; Afkhami, Abbas

    2015-08-01

    A sensitive spectrofluorimetric method using constant-energy synchronous fluorescence technique is proposed for the determination of human albumin without separation. In this method, no reagent was used for enhancement of the fluorescence signal of albumin in the solution. Effects of some parameters, such as energy difference between excitation and emission monochromators (ΔE), emission and excitation slit widths and scan rate of wavelength were studied and the optimum conditions were established. For this purpose factorial design and response surface method were employed for optimization of the effective parameters on the fluorescence signal. The results showed that the scan rate of the wavelength has no significant effect on the analytical signal. The calibration curve was linear in the range 0.1-220.0 µg mL(-1) of albumin with a detection limit of 7.0 × 10(-3)  µg mL(-1). The relative standard deviations (RSD) for six replicate measurements of albumin were calculated as 2.2%, 1.7% and 1.3% for 0.5, 10.0 and 100.0 µg mL(-1) albumin, respectively. Furthermore the proposed method has been employed for the determination of albumin in human serum and urine samples.

  9. Albumin to creatinine ratio in a random urine sample: Correlation with severity of preeclampsia

    Directory of Open Access Journals (Sweden)

    Fady S. Moiety

    2014-06-01

    Conclusions: Random urine ACR may be a reliable method for prediction and assessment of severity of preeclampsia. Using the estimated cut-off may add to the predictive value of such a simple quick test.

  10. Detection of Wuchereria bancrofti DNA in paired serum and urine samples using polymerase chain reaction-based systems

    Directory of Open Access Journals (Sweden)

    Camila Ximenes

    2014-12-01

    Full Text Available The Global Program for the Elimination of Lymphatic Filariasis (GPELF aims to eliminate this disease by the year 2020. However, the development of more specific and sensitive tests is important for the success of the GPELF. The present study aimed to standardise polymerase chain reaction (PCR-based systems for the diagnosis of filariasis in serum and urine. Twenty paired biological urine and serum samples from individuals already known to be positive for Wuchereria bancrofti were collected during the day. Conventional PCR and semi-nested PCR assays were optimised. The detection limit of the technique for purified W. bancrofti DNA extracted from adult worms was 10 fg for the internal systems (WbF/Wb2 and 0.1 fg by using semi-nested PCR. The specificity of the primers was confirmed experimentally by amplification of 1 ng of purified genomic DNA from other species of parasites. Evaluation of the paired urine and serum samples by the semi-nested PCR technique indicated only two of the 20 tested individuals were positive, whereas the simple internal PCR system (WbF/Wb2, which has highly promising performance, revealed that all the patients were positive using both samples. This study successfully demonstrated the possibility of using the PCR technique on urine for the diagnosis of W. bancrofti infection.

  11. Development of a rapid PCR assay specific for Staphylococcus saprophyticus and application to direct detection from urine samples.

    Science.gov (United States)

    Martineau, F; Picard, F J; Ménard, C; Roy, P H; Ouellette, M; Bergeron, M G

    2000-09-01

    Staphylococcus saprophyticus is one of the most frequently encountered microorganisms associated with acute urinary tract infections (UTIs) in young, sexually active female outpatients. Conventional identification methods based on biochemical characteristics can efficiently identify S. saprophyticus, but the rapidities of these methods need to be improved. Rapid and direct identification of this bacterium from urine samples would be useful to improve time required for the diagnosis of S. saprophyticus infections in the clinical microbiology laboratory. We have developed a PCR-based assay for the specific detection of S. saprophyticus. An arbitrarily primed PCR amplification product of 380 bp specific for S. saprophyticus was sequenced and used to design a set of S. saprophyticus-specific PCR amplification primers. The PCR assay was specific for S. saprophyticus when tested with DNA from 49 gram-positive and 31 gram-negative bacterial species. This assay was also able to amplify efficiently DNA from all 60 strains of S. saprophyticus from various origins tested. This assay was adapted for direct detection from urine samples. The sensitivity levels achieved with urine samples was 19 CFU with 30 cycles of amplification and 0.5 CFU with 40 cycles of amplification. This PCR assay for the specific detection of S. saprophyticus is simple and rapid (approximately 90 min, including the time for urine specimen preparation).

  12. Analysis of Drugs of Abuse in Anonymously Collected Urine and Soil samples from a Music Festival in Scandinavia

    DEFF Research Database (Denmark)

    Mardal, Marie; Ramin, Pedram; Plósz, Benedek G.

    and urine samples were also prepared by adding acetonitrile, shaking, centrifugation, and evaporation. Extracts were then analyzed by UHPLC-MSn (TF LXQ), UHPLC-HRMS/MS (TF Q-Exactive), and GC-MS (TF ISQ). Urine samples were additionally tested for 9-carboxy-THC by immunoassay and ethanol by headspace GC......, sertraline, and loperamide could be detected. 9-carboxy-THC was detected in most samples by immunoassay and confirmed by GC-MS; six thereof with immunoassay concentrations >50 ng/mL. The average ethanol concentration was 0.60 g/L ± 0.12 (α=0.05, n=21). In the soil samples, the following drugs of abuse could...

  13. Clenbuterol storage stability in the bovine urine and liver samples used for European official control in the azores islands (portugal).

    Science.gov (United States)

    Pinheiro, Isabel; Jesuino, Bruno; Barbosa, Jorge; Ferreira, Humberto; Ramos, Fernando; Matos, José; da Silveira, Maria Irene Noronha

    2009-02-11

    Clenbuterol is a well-known growth promoter, illegally used in farm animals, especially in cattle. Samples collected for the screening of beta(2)-agonist residues in Portuguese Azores Islands must travel through all the nine islands until they reach Azores Central Laboratory. If any suspicious sample is detected, it must be further transported to the National Reference Laboratory in Lisbon for confirmation. As a consequence of these circumstances, samples are submitted to different transport and storage times, as well as different temperature conditions and in some cases successive freezing and thawing cycles. As clenbuterol is the most detected beta(2)-agonist growth promoter in the Portuguese Residue Monitoring Plan, studies were conducted on the stability of this compound in incurred samples (bovine liver and urine) at +4, -20 and -60 degrees C over time. Samples kept at -20 degrees C were also analyzed over time after successive freezing and thawing cycles. The analyses of clenbuterol over time were performed by gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring (SIM). Clenbuterol in incurred urine and liver samples was significantly stable up to 20 weeks at -20 and -60 degrees C and after, at least, six consecutive freezings and thawings. At +4 degrees C, clenbuterol remained stable, at least until 12 weeks in urine and up to 20 weeks in liver.

  14. Temporal variability in urinary phthalate metabolite excretion based on spot, morning, and 24-h urine samples: Considerations for epidemiological studies

    DEFF Research Database (Denmark)

    Frederiksen, Hanne; Kranich, Selma K.; Jørgensen, Niels;

    2013-01-01

    Urinary phthalate excretion is used as marker of phthalate exposure in epidemiological studies. Here we examine the reliability of urinary phthalate levels in exposure classification by comparing the inter- and intrasubject variation of urinary phthalate metabolite levels. Thirty-three young...... healthy men each collected two spot, three first-morning, and three 24-h urine samples during a 3-month period. Samples were analyzed for the content of 12 urinary metabolites of 7 different phthalates. Variability was assessed as intraclass correlation coefficients (ICC). For the metabolites of diethyl...... of exposures for these two phthalates in population studies and hence an attenuation of the power to detect possible exposure-outcome associations. The only slightly higher ICCs for 24-h pools compared to first-morning and spot urine samples does not seem to justify the extra effort needed to collect 24-h...

  15. Comparative Evaluation of Inoculation of Urine Samples with the Copan WASP® and BD Kiestra™ InoqulA™ Instruments

    DEFF Research Database (Denmark)

    Iversen, Jesper; Stendal, Gitta; Gerdes, Cecilie Marie

    2016-01-01

    This study evaluated quantitative results as well as the quality of the inoculation patterns on urine specimens produced by two automated instruments, the Copan WASP® and the BD InoqulA™. 526 urine samples submitted in 10 ml canisters containing boric acid were processed within 30 minutes...... on an InoqulA, plating 10 ul of specimen, and two WASP instruments, one plating 1 ul of specimen (WASP-1) and the second WASP 10 ul (WASP-10). All samples were incubated, analysed, and digitally imaged using the BD Kiestra™ Total Lab Automation system. Results were evaluated using a quantitative protocol...... of the automated instruments divided by the counts for the calibrated pipet (golden standard). Ratios for the InoqulA were closest to 1,0 with the smallest standard deviations indicating that, compared to a calibrated pipet, the InoqulA results were more accurate than the WASP.. For clinical samples, the WASPs...

  16. Spectrophotometric and fluorimetric determination of diazepam, bromazepam and clonazepam in pharmaceutical and urine samples

    Science.gov (United States)

    Salem, A. A.; Barsoum, B. N.; Izake, E. L.

    2004-03-01

    New spectrophotometric and fluorimetric methods have been developed to determine diazepam, bromazepam and clonazepam (1,4-benzodiazepines) in pure forms, pharmaceutical preparations and biological fluid. The new methods are based on measuring absorption or emission spectra in methanolic potassium hydroxide solution. Fluorimetric methods have proved selective with low detection limits, whereas photometric methods showed relatively high detection limits. Successive applications of developed methods for drugs determination in pharmaceutical preparations and urine samples were performed. Photometric methods gave linear calibration graphs in the ranges of 2.85-28.5, 0.316-3.16, and 0.316-3.16 μg ml -1 with detection limits of 1.27, 0.08 and 0.13 μg ml -1 for diazepam, bromazepam and clonazepam, respectively. Corresponding average errors of 2.60, 5.26 and 3.93 and relative standard deviations (R.S.D.s) of 2.79, 2.12 and 2.83, respectively, were obtained. Fluorimetric methods gave linear calibration graphs in the ranges of 0.03-0.34, 0.03-0.32 and 0.03-0.38 μg ml -1 with detection limits of 7.13, 5.67 and 16.47 ng ml -1 for diazepam, bromazepam and clonazepam, respectively. Corresponding average errors of 0.29, 4.33 and 5.42 and R.S.D.s of 1.27, 1.96 and 1.14 were obtained, respectively. Statistical Students t-test and F-test have been used and satisfactory results were obtained.

  17. Urine sample preparation and fractionation for global proteome profiling by LC-MS.

    Science.gov (United States)

    Court, Magali; Garin, Jérôme; Masselon, Christophe D

    2015-01-01

    Urine has garnered tremendous interest over the past decade as a potential source of protein biomarkers for various pathologies. However, due to its low protein concentration and the presence of interfering compounds, urine constitutes a challenging analyte in proteomics. In the context of a project aimed at the discovery and evaluation of new candidate biomarkers of bladder cancer in urine, our laboratory has implemented and evaluated an array of preparation techniques for urinary proteome analysis. We present here the protocol that, in our hands, yielded the best overall proteome coverage with the lowest analytical effort. It begins with protein precipitation using trichloroacetic acid, in solution digestion and RP-C18 cartridge desalting of the resulting peptides mixture, and is followed by peptide fractionation by gel-free isoelectric focusing, and nano-LC-MS/MS for database compilation.

  18. Determination of Atto- to Femtogram Levels of Americium and Curium Isotopes in Large-Volume Urine Samples by Compact Accelerator Mass Spectrometry.

    Science.gov (United States)

    Dai, Xiongxin; Christl, Marcus; Kramer-Tremblay, Sheila; Synal, Hans-Arno

    2016-03-01

    Ultralow level analysis of actinides in urine samples may be required for dose assessment in the event of internal exposures to these radionuclides at nuclear facilities and nuclear power plants. A new bioassay method for analysis of sub-femtogram levels of Am and Cm in large-volume urine samples was developed. Americium and curium were co-precipitated with hydrous titanium oxide from the urine matrix and purified by column chromatography separation. After target preparation using mixed titanium/iron oxides, the final sample was measured by compact accelerator mass spectrometry. Urine samples spiked with known quantities of Am and Cm isotopes in the range of attogram to femtogram levels were measured for method evaluation. The results are in good agreement with the expected values, demonstrating the feasibility of compact accelerator mass spectrometry (AMS) for the determination of minor actinides at the levels of attogram/liter in urine samples to meet stringent sensitivity requirements for internal dosimetry assessment.

  19. Microchip in situ electrosynthesis of silver metallic oxide clusters for ultra-FAST detection of galactose in galactosemic newborns' urine samples.

    Science.gov (United States)

    García-Carmona, Laura; Rojas, Daniel; González, María Cristina; Escarpa, Alberto

    2016-10-17

    This work describes for the first time the coupling of microfluidic chips (MC) to electrosynthetized silver metallic oxide clusters (AgMOCs). As an early demonstration of this novel approach, the ultrafast detection of galactose in galactosemic newborns' urine samples is proposed. AgMOCs were in situ electrosynthetized on integrated microchip platinum electrodes using a double pulse technique and characterized in full using scanning electronic microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) and electrochemical techniques revealing the presence of silver oxides and electrocatalysis towards galactose as a galactosemia biomarker. Galactose detection in galactosemic newborns' urine samples proceeded in less than 30 s, differentiating between ill and healthy urine samples and requiring negligible urine sample consumption. The significance of the newborns' urine samples confirmed the analytical potency of the MC-AgMOCs approach for future implementation of screening for rare disease diagnosis such as galactosemia.

  20. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  1. Dynamic versus static ultrasonic sample treatment for the solid-liquid pre-concentration of mercury from human urine.

    Science.gov (United States)

    Patricio, A; Fernandez, C; Mota, A M; Capelo, J L

    2006-05-15

    Dynamic and static ultrasonic procedures involving ultrasonic bath and tandem focused ultrasound (i.e. two probes were used in the same sample treatment) have been assessed in order to implement a reliable solid-liquid back extraction of mercury from commercial resins (dowex and chelex-100), previously used to concentrate Hg(II) from treated urine. The urine had been previously treated with an advanced oxidation process provided by the conjunction of potassium permanganate, hydrochloric acid and high intensity focused ultrasound, which allowed that organic matter degradation was achieved in less than 3min. 95+/-10% of mercury in the certified urine and 97+/-6% of the spiked methyl-mercury was recovered with the dowex resin plus the static ultrasonic procedure, whilst 96+/-11% of the spiked mercury was recovered with the dowex resin plus the dynamic procedure, for which ultrasonication was not necessary. The Hg pre-concentration factor used in this work was 8 (20mL of urine to 2.5mL of acid), but different volume ratios can be used in order to increase this factor.

  2. Detection and sequencing of West Nile virus RNA from human urine and serum samples during the 2014 seasonal period.

    Science.gov (United States)

    Nagy, Anna; Bán, Enikő; Nagy, Orsolya; Ferenczi, Emőke; Farkas, Ágnes; Bányai, Krisztián; Farkas, Szilvia; Takács, Mária

    2016-07-01

    West Nile virus, a widely distributed mosquito-borne flavivirus, is responsible for numerous animal and human infections in Europe, Africa and the Americas. In Hungary, the average number of human infections falls between 10 and 20 cases each year. The severity of clinically manifesting infections varies widely from the milder form of West Nile fever to West Nile neuroinvasive disease (WNND). In routine laboratory diagnosis of human West Nile virus infections, serological methods are mainly applied due to the limited duration of viremia. However, recent studies suggest that detection of West Nile virus RNA in urine samples may be useful as a molecular diagnostic test for these infections. The Hungarian National Reference Laboratory for Viral Zoonoses serologically confirmed eleven acute human infections during the 2014 seasonal period. In three patients with neurological symptoms, viral RNA was detected from both urine and serum specimens, albeit for a longer period and in higher copy numbers with urine. Phylogenetic analysis of the NS3 genomic region of three strains and the complete genome of one selected strain demonstrated that all three patients had lineage-2 West Nile virus infections. Our findings reaffirm the utility of viral RNA detection in urine as a molecular diagnostic procedure for diagnosis of West Nile virus infections.

  3. Black Urine

    Directory of Open Access Journals (Sweden)

    Rahim Vakili

    2016-06-01

    Full Text Available A 2-year-old boy was born at term of healthy, non-consanguineous Iranian parents. His mother attended in the clinic with the history of sometimes discoloration of diapers after passing urine. She noticed that first at the age of one month with intensified in recent months. His Physical examination and growth parameters were normal. His mother denied taking any medication (sorbitol, nitrofurantoin, metronidazole, methocarbamol, sena and methyldopa (5. Qualitative urine examination showed dark black discoloration. By this history, alkaptonuria was the most clinical suspicious. A 24-hour-urine sample was collected and sent for quantitative measurements. The urine sample was highly positive for homogentisic acid and negative for porphyrin metabolites.

  4. Phthalate metabolites in urine samples from Danish children and correlations with phthalates in dust samples from their homes and daycare centers

    DEFF Research Database (Denmark)

    Langer, S.; Bekö, Gabriel; Weschler, Charles J.;

    2013-01-01

    Around the world humans use products that contain phthalates, and human exposure to certain of these phthalates has been associated with various adverse health effects. The aim of the present study has been to determine the concentrations of the metabolites of diethyl phthalate (DEP), di......(n-butyl) phthalate (DnBP), di(iso-butyl) phthalate (DiBP), butyl benzyl phthalate (BBzP) and di(2-ethylhexyl) phthalate (DEHP) in urine samples from 441 Danish children (3–6 years old). These children were subjects in the Danish Indoor Environment and Children's Health study. As part of each child's medical...... examination, a sample from his or her first morning urination was collected. These samples were subsequently analyzed for metabolites of the targeted phthalates. The measured concentrations of each metabolite were approximately log-normally distributed, and the metabolite concentrations significantly...

  5. Temporal variability in urinary excretion of bisphenol A and seven other phenols in spot, morning, and 24-h urine samples

    DEFF Research Database (Denmark)

    Lassen, Tina Harmer; Frederiksen, Hanne; Jensen, Tina Kold

    2013-01-01

    (ICCs). More than 70% of the urine samples had detectable levels of BPA, triclosan (TCS), benzophenone-3 (BP-3) and sum of 2,4-dichlorophenol and 2,5-dichlorophenol (σDCP). We found low to moderate ICCs for BPA (0.10-0.42) and σDCP (0.39-0.72), whereas the ICCs for BP-3 (0.69-0.80) and TCS (0...

  6. Rapid and sensitive determination of strychnine and brucine in human urine by capillary electrophoresis with field-amplified sample stacking.

    Science.gov (United States)

    Li, Junmei; Jiang, Ye

    2010-02-01

    A simple, rapid, sensitive and low-cost method using capillary electrophoresis (CE) coupled with field-amplified sample stacking (FASS) has been developed and validated for the simultaneous determination of strychnine and brucine residues in human urine. Before sample loading, a water plug (3.5 kPa, 3 s) was injected to contain sample cations and to permit FASS. Electrokinetic injection at a voltage (20 kV, 25 s) was then used to introduce cations. Separation was performed using 20 mM acetate buffer (pH 3.8) with an applied voltage of 20 kV. The calibration curves were linear over a range of 8.00-2.56 infinity 10(2) ng/mL (r = 0.9995) for strychnine and 10.0-3.20 x 10(2) ng/mL (r = 0.9999) for brucine. Extraction recoveries in urine were greater than 79.6 and 82.8% for strychnine and brucine, respectively, with an RSD of less than 4.9%. The detection limits (signal-to-noise ratio 3) for strychnine and brucine were 2.00 and 2.50 ng/mL, respectively. A urine sample from one healthy female volunteer (26 years old, 50 kg) was pretreated and analyzed. Strychnine and brucine levels in urine could be detected 24 h after administration. On these grounds, this method was feasible for application to preliminary screening of trace levels of abused drugs for both doping control and forensic analysis. (c) 2009 John Wiley & Sons, Ltd.

  7. Detection of dopamine in non-treated urine samples using glassy carbon electrodes modified with PAMAM dendrimer-Pt composites

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, M.G. [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico); Department of Chemistry, Universidad de Guanajuato, Cerro de la Venada S/N Col. Pueblito de Rocha, 36040 Guanajuato, Gto (Mexico); Armendariz, G.M.E.; Godinez, Luis A.; Torres, J. [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico); Sepulveda-Guzman, S. [Centro de Innovacion, Investigacion y Desarrollo en Ingenieria y Tecnologia, Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Universidad, San Nicolas de los Garza, Nuevo Leon, 66451 Nuevo Leon (Mexico); Bustos, E., E-mail: ebustos@cideteq.mx [Laboratory of Bioelectrochemistry, Centro de Investigacion y Desarrollo Tecnologico en Electroquimica, S. C., Parque Tecnologico, Queretaro, Sanfandila, Pedro Escobedo 76703, Queretaro (Mexico)

    2011-09-01

    Composites of hydroxyl-terminated PAMAM dendrimers, generation 4.0 (64 peripheral OH groups) containing Pt nanoparticles were synthesized at different reaction times using a microwave reactor. The synthetic procedure resulted in dendrimer encapsulated nanoparticles of Pt (DENs-Pt) of 1.53 {+-} 0.17 nm diameter that was calculated from transmission electron microscopy, and the Pt nanoparticles had single crystal plane in (1 1 1) orientation determinate by selective area diffraction. Each composite was electrochemically immobilized on a pre-functionalized glassy carbon (GC) electrode that was incorporated as a flow injection amperometric (FIA) detector, for the selective detection and quantification of dopamine (DA) in untreated urine samples. Comparison of the analytical performance of the novel electrochemical detector revealed that the DENs-Pt modified GC electrode with the composite synthesized for 30 min in the microwave reactor, showed the best response for the detection of DA in samples of non-treated urine, being the detection and quantification limits smaller (19 and 9 ppb, respectively) than those corresponding to the naked a GC electrode (846 and 423 ppb, respectively) using the FIA detector. In addition, it was found that this electroanalytical approach suffers minimal matrix effects that arise in the analysis of DA in untreated samples of urine.

  8. Antimicrobial resistance in Escherichia coli isolated from bitches with pyometra and from urine samples from other dogs.

    Science.gov (United States)

    Hagman, R; Greko, C

    2005-08-13

    To assess whether the rates of antimicrobial susceptibility in bacteria isolated from the urine of dogs with urinary tract infections are similar to those of bacteria isolated from bitches with pyometra, the antimicrobial resistance of Escherichia coli isolated from the two groups were determined and compared. The samples were collected in Sweden between April 2002 and March 2003, and potential changes over time were assessed by comparing the results with corresponding data from 1991 to 1993. Among 80 isolates of E coli from cases of pyometra, the proportions that were resistant to the antimicrobials used in canine practice were generally low (ampicillin 10 per cent, enrofloxacin 4 per cent, gentamicin 0 per cent, streptomycin 5 per cent, sulfamethoxazole 8 per cent, tetracycline 4 per cent and trimethoprim 2 per cent) and similar to the proportions reported previously. Significantly lower proportions of resistance were recorded among the pyometra isolates than among 92 isolates from urine samples submitted by animal hospitals to ampicillin (P=0.04), streptomycin (P=0.002) and tetracycline (P=0.03), but there were no differences between the pyometra isolates and 113 isolates from urine samples submitted by animal clinics.

  9. Photoluminescence of urine salts

    Science.gov (United States)

    Bordun, O.; Drobchak, O.

    2008-02-01

    Photoexcitation and luminescence spectra of dried urine sample under laser excitation were studied. Luminescence spectra of urine are determined by luminescence of urea which is the main component of urine. The presence of pathological salts in urine leads to the long-wave shifting of maxima of luminescence and to the decreasing of luminescence intensity.

  10. Evaluation of the BinaxNOW® Streptococcus pneumoniae antigen test on fresh, frozen and concentrated urine samples in elderly patients with and without community-acquired pneumonia.

    Science.gov (United States)

    Saukkoriipi, Annika; Pascal, Thierry; Palmu, Arto A

    2016-02-01

    We evaluated the BinaxNOW® urine antigen test in elderly. For fresh un-concentrated urine samples, the sensitivity for pneumococcal pneumonia was 63% and specificity 97%. After freezing and concentration, the results comparable to positive control line in intensity at 60 min gave high sensitivity (81%) with no loss in specificity (96%).

  11. Candida colonization in urine samples of ICU patients: determination of etiology, antifungal susceptibility testing and evaluation of associated risk factors.

    Science.gov (United States)

    Singla, Nidhi; Gulati, Neelam; Kaistha, Neelam; Chander, Jagdish

    2012-08-01

    The presence of Candida in urine presents a therapeutic challenge for the physician as it is often asymptomatic, and management guidelines have not been clearly laid down on this issue. The presence of Candida in urine may represent contamination of clinical sample, actual colonization of the lower urinary tract or may be a true indicator of invasive infection of lower and/or upper urinary tract. In a clinical setting like the ICU, multiple risk factors for Candida colonization may be present in the same patient, thereby increasing the chances of candiduria, manifold. In the present study on 80 patients in ICU, high rate of Candida colonization (57.5%) was found in urine samples of ICU patients with C. tropicalis (57.3%) being the predominant species. We also isolated 8 strains of Trichosporon species, all of these presented as a mixed infection along with Candida species. Among the various risk factors studied, urinary catheterization and previous antibiotic therapy were identified as statistically significant (P value albicans, C. glabrata and Trichosporon species, respectively.

  12. Structural Elucidation of a Carnosine-Acrolein Adduct and its Quantification in Human Urine Samples.

    Science.gov (United States)

    Bispo, Vanderson S; de Arruda Campos, Ivan P; Di Mascio, Paolo; Medeiros, Marisa H G

    2016-01-19

    Aldehydes accumulate in inflammation, during myocardial infarction and have been associated with pain symptoms. One pathway of aldehyde detoxification is the conjugation with carnosine. A 3-methylpyridinium carnosine adduct from the reaction of carnosine and acrolein was characterized using extensive spectroscopic measurements. The adduct with urinary concentrations of 1.82 ± 0.68 nmol/mg of creatinine is one of the most abundant acrolein metabolites in urine and opens promising therapeutic strategies for carnosine.

  13. Intercomparison run for uranium and tritium determination in urine samples, organised by Nuclear Regulatory Authority, Argentina

    CERN Document Server

    Serdeiro, N H; Equillor, H E

    2003-01-01

    The Nuclear Regulatory Authority (ARN), Argentina, has carried out an intercomparison run for tritium and uranium determination in urine, in November 2002. The aim of this exercise was to assess the performance of the laboratories that usually inform these radionuclides and to provide technical support in order to have an appropriate occupational monitoring in vitro. In the present work, the results of the intercomparison and the assessment of each laboratory are published.

  14. The urine marker test

    DEFF Research Database (Denmark)

    Elbe, Anne-Marie; Jensen, Stine Nylandsted; Elsborg, Peter

    2016-01-01

    BACKGROUND: Urine sample collection for doping control tests is a key component of the World Anti-Doping Agency's fight against doping in sport. However, a substantial number of athletes experience difficulty when having to urinate under supervision. Furthermore, it cannot always be ensured...... that athletes are actually delivering their own urine. A method that can be used to alleviate the negative impact of a supervised urination procedure and which can also identify urine as coming from a specific athlete is the urine marker test. Monodisperse low molecular weight polyethylene glycols (PEGs......) are given orally prior to urination. Urine samples can be traced to the donor by analysis of the PEGs previously given. OBJECTIVE: The objective of this study was to investigate the use of the urine marker during urine doping control testing. METHODS: Two studies investigated athletes' acceptance...

  15. Multiple stage MS in analysis of plasma, serum, urine and in vitro samples relevant to clinical and forensic toxicology.

    Science.gov (United States)

    Meyer, Golo M; Maurer, Hans H; Meyer, Markus R

    2016-01-01

    This paper reviews MS approaches applied to metabolism studies, structure elucidation and qualitative or quantitative screening of drugs (of abuse) and/or their metabolites. Applications in clinical and forensic toxicology were included using blood plasma or serum, urine, in vitro samples, liquids, solids or plant material. Techniques covered are liquid chromatography coupled to low-resolution and high-resolution multiple stage mass analyzers. Only PubMed listed studies published in English between January 2008 and January 2015 were considered. Approaches are discussed focusing on sample preparation and mass spectral settings. Comments on advantages and limitations of these techniques complete the review.

  16. Direct trace-elemental analysis of urine samples by laser ablation-inductively coupled plasma mass spectrometry after sample deposition on clinical filter papers.

    Science.gov (United States)

    Aramendía, Maite; Rello, Luis; Vanhaecke, Frank; Resano, Martín

    2012-10-16

    Collection of biological fluids on clinical filter papers shows important advantages from a logistic point of view, although analysis of these specimens is far from straightforward. Concerning urine analysis, and particularly when direct trace elemental analysis by laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS) is aimed at, several problems arise, such as lack of sensitivity or different distribution of the analytes on the filter paper, rendering obtaining reliable quantitative results quite difficult. In this paper, a novel approach for urine collection is proposed, which circumvents many of these problems. This methodology consists on the use of precut filter paper discs where large amounts of sample can be retained upon a single deposition. This provides higher amounts of the target analytes and, thus, sufficient sensitivity, and allows addition of an adequate internal standard at the clinical lab prior to analysis, therefore making it suitable for a strategy based on unsupervised sample collection and ulterior analysis at referral centers. On the basis of this sampling methodology, an analytical method was developed for the direct determination of several elements in urine (Be, Bi, Cd, Co, Cu, Ni, Sb, Sn, Tl, Pb, and V) at the low μg L(-1) level by means of LA-ICPMS. The method developed provides good results in terms of accuracy and LODs (≤1 μg L(-1) for most of the analytes tested), with a precision in the range of 15%, fit-for-purpose for clinical control analysis.

  17. Comparison of individual and pooled urine samples for estimating the presence and intensity of Schistosoma haematobium infections at the population level.

    Science.gov (United States)

    Degarege, Abraham; Erko, Berhanu; Mekonnen, Zeleke; Legesse, Mengistu; Negash, Yohannes; Vercruysse, Jozef; Levecke, Bruno

    2015-11-16

    There is a lack of cost-effective diagnostic strategies to evaluate whether mass drug administration (MDA) programmes to control Schistosoma haematobium progress as anticipated. The purpose of this study is to provide a proof-of-principle for examination of pooled urine samples as a strategy for rapid assessment of presence and intensity of Schistosoma haematobium infections at the population level. A total of 640 urine samples were collected from 520 school-aged children (520 at baseline and 120 at follow-up) during a clinical trial that was designed to assess the efficacy of praziquantel against Schistosoma haematobium infections in Ethiopia. Individual and pooled urine samples were screened using the filtration technique (volume of 10 ml urine) to determine the number of S. haematobium eggs in 10 ml of urine. Samples were pooled into pools of 5 (n = 128), 10 (n = 64) and 20 (n = 32) individual samples. The sensitivity, the probability of finding at least one egg in a pooled sample when the mean urine egg count (UEC) of the corresponding individual urine samples was not zero, was calculated for each pool size. UECs of a pooled examination strategy were compared with the mean UECs of the corresponding individual samples. The sensitivity of a pooled examination strategy was 50.6% for pools of 5, 68.6% for pools of 10 and 63.3% for pools of 20. The sensitivity of a pooled examination strategy increased as a function of increasing mean UEC of the corresponding individual urine samples. For each of the three pool sizes, there was a significant positive correlation between mean UECs of individual and those obtained in pooled samples (correlation coefficient: 0.81 - 0.93). Examination of pools of 5 provided significantly lower UECs compared to the individual examination strategy (3.9 eggs/10 ml urine versus 5.0 eggs/10 ml urine). For pools of 10 (4.4 eggs/10 ml) and 20 (4.2 eggs/10 ml), no significant difference in UECs was observed. Examination of pooled

  18. Rapid screening method for determination of Ecstasy and amphetamines in urine samples using gas chromatography-chemical ionisation mass spectrometry.

    Science.gov (United States)

    Pellegrini, M; Rosati, F; Pacifici, R; Zuccaro, R; Romolo, F S; Lopez, A

    2002-04-05

    The need for analytical screening tests more reliable and valid to detect amphetamine and related "designer drugs" in biological samples is becoming critical, due to the increasing diffusion of these drugs on the European illegal market. The most common screening procedures based on immunoassays suffer a number of limitations, including low sensitivity, lack of specificity and limited number of detectable substances. This paper describes a screening method based on gas-chromatography-mass-spectrometry (GC/MS) using positive chemical ionisation (PCI) detection. Methanol was used as reactant gas in the ionisation chamber. Molecular ions of different compounds were monitored, allowing a sensitivity of 5-10 ng/ml with high selectivity. The sensitivity of the method gives positive results in samples taken 48-72 h after intake of one dose of 50-100 mg. The method is simple and rapid. Sample preparation was limited to one liquid-liquid extraction, without any hydrolysis and derivatisation. Hydrolysis is critical to identify metabolites excreted as conjugates. Blank urine samples spiked with known amounts of amphetamine (AM), methylamphetamine (MA), methylenedioxyamphetamine (MDA), methylenedioxymethylamphetamine (MDMA), methylenedioxyethylamphetamine (MDEA) and methylenedioxyphenyl-N-methyl-2-butanamine (MBDB) were analysed. The method was successfully tested on real samples of urine from people, whose use of amphetamine was suspected, and results were compared with results obtained with immunoassays.

  19. Profiles of urine samples taken from Ecstasy users at Rave parties: analysis by immunoassays, HPLC, and GC-MS.

    Science.gov (United States)

    Zhao, H; Brenneisen, R; Scholer, A; McNally, A J; ElSohly, M A; Murphy, T P; Salamone, S J

    2001-01-01

    The abuse of the designer amphetamines such as 3,4-methylenedioxymethamphetamine (MDMA, Ecstasy) is increasing throughout the world. They have become popular drugs, especially at all-night techno dance parties (Raves), and their detection is becoming an important issue. Presently, there are no MDMA- or MDA-specific immunoassays on the market, and detection of the designer amphetamines is dependent upon the use of commercially available amphetamine assays. The success of this approach has been difficult to assess because of the general unavailability of significant numbers of samples from known drug users. The objectives of the present study are to characterize the drug content of urine samples from admitted Ecstasy users by chromatographic methods and to assess the ability of the available amphetamine/methamphetamine immunoassays to detect methylenedioxyamphetamines. We found that, when analyzed by high-performance liquid chromatography with diode-array detection (HPLC-DAD), 64% of 70 urine samples (by gas chromatography-mass spectrometry [GC-MS]: 88% of 64 urine samples) obtained from Rave attendees contained MDMA and/or 3,4-methylenedioxyamphetamine (MDA) alone or in combination with amphetamine, methamphetamine, or other designer amphetamines such as 3,4-methylenedioxyethylamphetamine (MDEA). This suggests that the majority of the Ravers are multidrug users. At the manufacturer's suggested cutoffs, the Abbott TDx Amphetamine/Methamphetamine II and the new Roche HS Amphetamine/MDMA assays demonstrated greater detection sensitivity for MDMA than the other amphetamine immunoassays tested (Abuscreen OnLine Hitachi AMPS, Abuscreen OnLine Integra AMPS, Abuscreen OnLine Integra AMPSX, CEDIA AMPS, and EMIT II AMPS). There is 100% agreement between each of the two immunoassays with the reference chromatographic methods, HPLC-DAD and GC-MS, for the detection of methylenedioxyamphetamines.

  20. Novel method for simultaneous aqueous in situ derivatization of THC and THC-COOH in human urine samples: validation and application to real samples.

    Science.gov (United States)

    Chericoni, S; Battistini, I; Dugheri, S; Pacenti, M; Giusiani, M

    2011-05-01

    The present work describes the validation of a novel aqueous in situ derivatization procedure with trimethyloxonium tetrafluoroborate (TMO) as methylating agent for the simultaneous, quantitative analysis of Δ(9)-tetrahydrocannabinol (THC) and 11-nor-Δ(9)-tetrahydrocannabinol carboxylic acid (THC-COOH) in human urine. The derivatizing agent is directly added to the urine sample and the methyl-derivatives are then recovered by liquid-liquid extraction procedure. Gas chromatography-mass spectrometry was used to detect the derivatives in selected ion monitoring mode. The limits of detection were 0.7 ng/mL for THC and 0.5 ng/mL for THC-COOH, whereas the limits of quantification were 1.9 and 0.9 ng/mL, respectively. The method has been applied to 60 real samples both positive and negative to immunochemical screening test resulting to be very useful and reliable in routine analysis of THC-COOH in human urine for toxicological and forensic purposes.

  1. Magnetic nano graphene oxide as solid phase extraction adsorbent coupled with liquid chromatography to determine pseudoephedrine in urine samples.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed; Ebrahimi, Mahmoud

    2016-01-15

    This paper reports on a method based on magnetic solid phase extraction (MSPE) for the determination of pseudoephedrine. Magnetic nanographene oxide (MNGO) was applied as a new adsorbent for the extraction of pseudoephedrine from urine samples. Synthesis of MNGO was characterized by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and vibrating sample magnetometer (VSM). The main factors influencing extraction efficiency, including the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, ionic strength of extraction medium, and agitation rate, were investigated and optimized. Under optimized extraction conditions, a good linearity was observed in the range of 100-2000ng/mL with a correlation coefficient of 0.9908 (r(2)). Limit of detection (LOD) and limit of quantification (LOQ) were 25 and 82.7ng/mL, respectively. Inter-day and intra-day precision and accuracy were 6.01 and 0.34 (%), and 8.70 and 0.29 (%), respectively. The method was applied for the determination of pseudoephedrine in urine samples of volunteers receiving pseudoephedrine with the recovery of 96.42. It was concluded that the proposed method can be applied in diagnostic clinics.

  2. Application and Uses of Electronic Noses for Clinical Diagnosis on Urine Samples: A Review

    Science.gov (United States)

    Capelli, Laura; Taverna, Gianluigi; Bellini, Alessia; Eusebio, Lidia; Buffi, Niccolò; Lazzeri, Massimo; Guazzoni, Giorgio; Bozzini, Giorgio; Seveso, Mauro; Mandressi, Alberto; Tidu, Lorenzo; Grizzi, Fabio; Sardella, Paolo; Latorre, Giuseppe; Hurle, Rodolfo; Lughezzani, Giovanni; Casale, Paolo; Meregali, Sara; Sironi, Selena

    2016-01-01

    The electronic nose is able to provide useful information through the analysis of the volatile organic compounds in body fluids, such as exhaled breath, urine and blood. This paper focuses on the review of electronic nose studies and applications in the specific field of medical diagnostics based on the analysis of the gaseous headspace of human urine, in order to provide a broad overview of the state of the art and thus enhance future developments in this field. The research in this field is rather recent and still in progress, and there are several aspects that need to be investigated more into depth, not only to develop and improve specific electronic noses for different diseases, but also with the aim to discover and analyse the connections between specific diseases and the body fluids odour. Further research is needed to improve the results obtained up to now; the development of new sensors and data processing methods should lead to greater diagnostic accuracy thus making the electronic nose an effective tool for early detection of different kinds of diseases, ranging from infections to tumours or exposure to toxic agents. PMID:27754437

  3. Metabolomics identifies a biological response to chronic low-dose natural uranium contamination in urine samples.

    Science.gov (United States)

    Grison, Stéphane; Favé, Gaëlle; Maillot, Matthieu; Manens, Line; Delissen, Olivia; Blanchardon, Eric; Banzet, Nathalie; Defoort, Catherine; Bott, Romain; Dublineau, Isabelle; Aigueperse, Jocelyne; Gourmelon, Patrick; Martin, Jean-Charles; Souidi, Maâmar

    2013-01-01

    Because uranium is a natural element present in the earth's crust, the population may be chronically exposed to low doses of it through drinking water. Additionally, the military and civil uses of uranium can also lead to environmental dispersion that can result in high or low doses of acute or chronic exposure. Recent experimental data suggest this might lead to relatively innocuous biological reactions. The aim of this study was to assess the biological changes in rats caused by ingestion of natural uranium in drinking water with a mean daily intake of 2.7 mg/kg for 9 months and to identify potential biomarkers related to such a contamination. Subsequently, we observed no pathology and standard clinical tests were unable to distinguish between treated and untreated animals. Conversely, LC-MS metabolomics identified urine as an appropriate biofluid for discriminating the experimental groups. Of the 1,376 features detected in urine, the most discriminant were metabolites involved in tryptophan, nicotinate, and nicotinamide metabolic pathways. In particular, N-methylnicotinamide, which was found at a level seven times higher in untreated than in contaminated rats, had the greatest discriminating power. These novel results establish a proof of principle for using metabolomics to address chronic low-dose uranium contamination. They open interesting perspectives for understanding the underlying biological mechanisms and designing a diagnostic test of exposure.

  4. A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples

    Directory of Open Access Journals (Sweden)

    Reddy I

    2009-01-01

    Full Text Available Objective: The use of performance enhancing substances is banned in sports by the World Anti-Doping Agency (WADA. Though most prohibited substances can be detected by GC/MS, inclusion of corticosteroids and designer drugs has made it essential to detect these critical doping agents on LC/MS/MS due to their better separation and detection. Materials and Methods: A common extraction procedure for the isolation of acidic, basic and neutral drugs from urine samples was developed. A total of 28 doping drugs were analyzed on API 3200 Triple quadrupole mass spectrometer using C18 column in atmospheric pressure electrospray ionization. The mobile phase composition was a mixture of 1% formic acid and acetonitrile with gradient time period. Results: The method developed was very sensitive for detection of 28 doping agents. The linearity was performed for each drug and the total recovery percentage ranged from 57 to 114. Limit of detection is found to be 0.5 ng/ml for carboxy finasteride and 1-5 ng/ml for other drugs. The method was successfully used to detect positive urine samples of 3-OH-stanozolol, methyl phenidate, mesocarb, clomiphene metabolite and carboxy finasteride. Conclusion: The method developed based on controlled pH extraction method and HPLC-mass spectrometry analysis allowed better identification and confirmation of glucocorticosteroids and a few other drugs in different categories. The validated method has been used successfully for testing of 1000 In-competition samples. The method helped in detection of chemically and pharmacologically different banned drugs in urine in a single short run at a minimum required performance limit set by WADA.

  5. Assessing the potential for racial bias in hair analysis for cocaine: examining the relative risk of positive outcomes when comparing urine samples to hair samples.

    Science.gov (United States)

    Mieczkowski, Tom

    2011-03-20

    This article examines the conjecture that hair analysis, performed to detect cocaine use or exposure, is biased against African Americans. It does so by comparing the outcomes of 33,928 hair and 105,792 urine samples collected from both African American and white subjects. In making this comparison the analysis seeks to determine if there is a departure in rates of positive and negative outcomes when comparing the results of hair analysis for cocaine to the results from urinalysis for cocaine by racial group. It treats urine as an unbiased test. It compares both the relative ratios of positive outcomes when comparing the two groups and it calculates the relative risk of outcomes for each group for having positive or negative outcomes. The findings show that the ratios of each racial group are effectively same for hair and urine assays, and they also show that the relative risk and risk estimates for positive and negative outcomes are the same for both racial groups. Considering all samples, the cocaine positive risk estimate for the hair samples comparing the two racial groups is 3.28 and for urinalysis the risk estimate is 3.10 (Breslow-Day χ(2) .250, 1 df, p = 0.617) a non-significant difference in risk. For pre-employment samples, the cocaine positive risk estimate for the hair samples comparing the two racial groups is 3.10 and for urinalysis the risk estimate is 2.90 (Breslow-Day χ(2) .281, df = 1, p = 0.595), also a non-significant difference in risk.

  6. Determination of cadmium and lead in urine samples after dispersive solid–liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R.M.; Herrero Latorre, C., E-mail: carlos.herrero@usc.es

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L{sup −1}, respectively, and for Pb these limits were 0.13 and 0.43 μg L{sup −1}. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96–102% obtained for Cd and 97–101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE–SS–ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained. - Highlights: • Cd and Pb determination based on the combination of DSP, SS and ETAAS • Urine matrix was eliminated using DSPE based on multiwalled carbon nanotubes. • Slurry sampling technique permitted the direct injection of sample into the ETAAS atomizer.

  7. Extractive determination of ephedrine hydrochloride and bromhexine hydrochloride in pure solutions, pharmaceutical dosage form and urine samples.

    Science.gov (United States)

    Abdel-Ghani, N T; Rizk, M S; Mostafa, M

    2013-07-01

    Simple, rapid, sensitive, precise and accurate spectrophotometeric methods for the determination of ephedrine hydrochloride (E-HCl) and bromhexine hydrochloride (Br-HCl) in bulk samples, dosage form and in spiked urine samples were investigated. The methods are based on the formation of a yellow colored ion-associates due to the interaction between the examined drugs with picric acid (PA), chlorophyllin coppered trisodium salt (CLPH), alizarin red (AR) and ammonium reineckate (Rk) reagents. A buffer solution had been used and the extraction was carried out using organic solvent, the ion associates exhibit absorption maxima at 410, 410, 430 and 530 nm of (Br-HCl)with PA, CLPH, AR and Rk respectively; 410, 410, 435 and 530 of (E-HCl) with PA, CLPH, AR and Rk respectively. (E-HCl) and (Br-HCl) could be determined up to 13, 121, 120 and 160; 25, 200, 92 and 206 μg mL(-1), using PA, CLPH, AR and Rk respectively. The optimum reaction conditions for quantitative analysis were investigated. In addition, the molar absorptivity, Sandell sensitivity were determined for the investigated drug. The correlation coefficient was ≥0.995 (n=6) with a relative standard deviation (RSD) ≤1.15 for five selected concentrations of the reagents. Therefore the concentration of Br-HCl and E-HCl drugs in their pharmaceutical formulations and spiked urine samples had been determined successfully.

  8. Quantitation of anticancer drugs – Cyclophosphamide and ifosfamide in urine and water sewage samples by gas chromatography–mass spectrometry

    Directory of Open Access Journals (Sweden)

    Veeravan Lekskulchai

    2016-10-01

    Full Text Available Objectives: Cyclophosphamide (CP and ifosfamide (IF are effective anti-cancer drugs but their genotoxicity can harm everyone contacting them occupationally or environmentally. Therefore, a sensitive method for monitoring their amounts in biological and environmental samples is needed. This has aimed to develop a method for analyzing these drugs in urine and water sewage samples. Material and Methods: The drug spiked samples were extracted, derivatized, and analyzed by gas chromatography–mass spectrometry and the analytical parameters were validated. Results: The method gave linear calibration curves at the concentrations of 0–190 nmol/l. It had the quantitation limit of 3.8 nmol/l and showed acceptable specificity, accuracy, recovery and precision. Conclusions: The developed method can be used reliably for monitoring CP and IF concentrations in urine and water sewage. The method will be applied for preventing health risk from occupational and environmental exposures to these drugs. Int J Occup Med Environ Health 2016;29(5:815–822

  9. Development of an ultrasensitive immunochromatographic assay (ICA) strip for the rapid detection of phenylethanolamine A in urine and pork samples.

    Science.gov (United States)

    Junhua, Li; Chunsheng, Li; Meng, Wu; Yan, Zhang; Xiaofei, Ma; Hua, Cheng; Jinghui, Yan

    2015-04-01

    In this study a one-step immunochromatographic assay based on competitive format was developed for the rapid detection of phenylethanolamine A (PEAA) residues in urine and pork samples. A monoclonal antibody against PEAA was produced from BALB/c mice immunized with the PEAA-BSA conjugate. The results of this qualitative test strip were to be interpreted visually. The visual detection limit (VDL) and threshold level of the optimized immunochromatographic assay for PEAA were 0.1 ng/mL and 0.5 ng/mL, respectively. Cross-reactions with other β-agonists were not significant inhibitions to the performance of the test strip assay. The results from the test strip were in a good agreement with those obtained using a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) assay. The immunochromatographic assay developed here was a useful on-site screening tool that is rapid to use, low in cost, and extremely convenient for the detection of PEAA in urine samples and pork samples.

  10. Extractive determination of ephedrine hydrochloride and bromhexine hydrochloride in pure solutions, pharmaceutical dosage form and urine samples

    Science.gov (United States)

    Abdel-Ghani, N. T.; Rizk, M. S.; Mostafa, M.

    2013-07-01

    Simple, rapid, sensitive, precise and accurate spectrophotometeric methods for the determination of ephedrine hydrochloride (E-HCl) and bromhexine hydrochloride (Br-HCl) in bulk samples, dosage form and in spiked urine samples were investigated. The methods are based on the formation of a yellow colored ion-associates due to the interaction between the examined drugs with picric acid (PA), chlorophyllin coppered trisodium salt (CLPH), alizarin red (AR) and ammonium reineckate (Rk) reagents. A buffer solution had been used and the extraction was carried out using organic solvent, the ion associates exhibit absorption maxima at 410, 410, 430 and 530 nm of (Br-HCl)with PA, CLPH, AR and Rk respectively; 410, 410, 435 and 530 of (E-HCl) with PA, CLPH, AR and Rk respectively. (E-HCl) and (Br-HCl) could be determined up to 13, 121, 120 and 160; 25, 200, 92 and 206 μg mL-1, using PA, CLPH, AR and Rk respectively. The optimum reaction conditions for quantitative analysis were investigated. In addition, the molar absorptivity, Sandell sensitivity were determined for the investigated drug. The correlation coefficient was ⩾0.995 (n = 6) with a relative standard deviation (RSD) ⩽1.15 for five selected concentrations of the reagents. Therefore the concentration of Br-HCl and E-HCl drugs in their pharmaceutical formulations and spiked urine samples had been determined successfully.

  11. Hollow-fiber micro-extraction combined with HPLC for the determination of sitagliptin in urine samples

    Directory of Open Access Journals (Sweden)

    Rezaee Raheme

    2015-01-01

    Full Text Available This study successfully developed a three-phase hollow-fiber liquid phase micro extraction coupled with high performance liquid chromatography for determination of trace levels of an anti-diabetic drug, sitagliptin (STG, in urine samples. Sitagliptin was extracted from 15 mL of the basic sample solution with a pH of 8.5 into an organic extracting solvent (n-octanol impregnated in the pores of a hollow fiber and then back extracted into an acidified aqueous solution in the lumen of the hollow fiber with a pH of 3. After extraction, 20 µL of the acceptor phase was injected into HPLC. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME including pH of the source and receiving phases, type of organic phase, ionic strength, stirring rate, extraction time, the volume ratio of donor phase to acceptor phase and temperature were studied and optimized. Under the optimized conditions, enrichment factors up to 88 were achieved and the relative standard deviation of the method was in the range of 3 % to 6%. The results indicated that HF-LPME method has an excellent clean-up capacity and a high preconcentration factor and can serve as a simple and sensitive method for monitoring the drug in the urine samples.

  12. A needle extraction utilizing a molecularly imprinted-sol-gel xerogel for on-line microextraction of the lung cancer biomarker bilirubin from plasma and urine samples.

    Science.gov (United States)

    Moein, Mohammad Mahdi; Jabbar, Dunia; Colmsjö, Anders; Abdel-Rehim, Mohamed

    2014-10-31

    In the present work, a needle trap utilizing a molecularly imprinted sol-gel xerogel was prepared for the on-line microextraction of bilirubin from plasma and urine samples. Each prepared needle could be used for approximately one hundred extractions before it was discarded. Imprinted and non-imprinted sol-gel xerogel were applied for the extraction of bilirubin from plasma and urine samples. The produced molecularly imprinted sol-gel xerogel polymer showed high binding capacity and fast adsorption/desorption kinetics for bilirubin in plasma and urine samples. The adsorption capacity of molecularly imprinted sol-gel xerogel polymer was approximately 60% higher than that of non-imprinted polymer. The effect of the conditioning, washing and elution solvents, pH, extraction time, adsorption capacity and imprinting factor were investigated. The limit of detection and the lower limit of quantification were set to 1.6 and 5nmolL(-1), respectively using plasma or urine samples. The standard calibration curves were obtained within the concentration range of 5-1000nmolL(-1) in both plasma and urine samples. The coefficients of determination values (R(2)) were ≥0.998 for all runs. The extraction recovery was approximately 80% for BR in the human plasma and urine samples.

  13. Determination of cadmium and lead in urine samples after dispersive solid-liquid extraction on multiwalled carbon nanotubes by slurry sampling electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Álvarez Méndez, J.; Barciela García, J.; García Martín, S.; Peña Crecente, R. M.; Herrero Latorre, C.

    2015-04-01

    A new method for the determination of Cd and Pb in urine samples has been developed. The method involves dispersive solid-phase extraction (DSPE), slurry sampling (SS), and subsequent electrothermal atomic absorption spectrometry (ETAAS). Oxidized multiwalled carbon nanotubes (MWCNTs) were used as the sorbent material. The isolated MWCNT/analyte aggregates were treated with nitric acid to form a slurry and both metals were determined directly by injecting the slurry into the ETAAS-atomizer. The parameters that influence the adsorption of the metals on MWCNTs in the DSPE process, the formation and extraction of the slurry, and the ETAAS conditions were studied by different factorial design strategies. The detection and quantification limits obtained for Cd under optimized conditions were 9.7 and 32.3 ng L- 1, respectively, and for Pb these limits were 0.13 and 0.43 μg L- 1. The preconcentration factors achieved were 3.9 and 5.4. The RSD values (n = 10) were less than 4.1% and 5.9% for Cd and Pb, respectively. The accuracy of the method was assessed in recovery studies, with values in the range 96-102% obtained for Cd and 97-101% for Pb. In addition, the analysis of certified reference materials gave consistent results. The DSPE-SS-ETAAS method is a novel and useful strategy for the determination of Pb and Cd at low levels in human urine samples. The method is sensitive, fast, and free of matrix interferences, and it avoids the tedious and time-consuming on-column adsorption and elution steps associated with commonly used SPE procedures. The proposed method was used to determine Cd and Pb in urine samples of unexposed healthy people and satisfactory results were obtained.

  14. Association between aflatoxin M1 excreted in human urine samples with the consumption of milk and dairy products.

    Science.gov (United States)

    Mohd Redzwan, Sabran; Rosita, Jamaluddin; Mohd Sokhini, Abdul Mutalib; Nurul Aqilah, Abdul Rahman

    2012-12-01

    This study aimed to find the association between urinary aflatoxin M(1) level and milk and dairy products consumption. Of 160 morning urine samples collected, aflatoxin M(1) was detected in 61.3 % samples (n = 98) [mean ± SD = 0.0234 ± 0.0177 ng/mL; range = 0-0.0747 ng/mL]. Of these positive samples, 67.3 % (n = 66) had levels above the limit of detection. Respondents with intake of milk and dairy products above median (67.79 g/day) had significantly high level of AFM(1) compared to those with low intake. A significant and positive association (φ = 0.286) was found between milk and dairy products consumption and urinary aflatoxin M(1) level.

  15. [Twenty-four hour time and frequency domain variability of systolic blood pressure and heart rate in an experimental model of arterial hypertension plus obesity].

    Science.gov (United States)

    Pelat, M; Verwaerde, P; Lazartiques, E; Cabrol, P; Galitzky, J; Berlan, M; Montastruc, J L; Senard, J M

    1998-08-01

    Modifications of heart rate (HR) and systolic blood pressure (SBP) variabilities (V) have been reported in the human syndrome arterial hypertension plus insulin-resistance. The aim of this study was to characterize the 24 h SBPV and HRV in both time and frequency domains during weight increase in dogs fed ad libitum with a high fat diet. Implantable transmitter units for measurement of blood pressure and heart rate were surgically implanted in five beagle male dogs. BP and HR were continuously recorded using telemetric measurements during 24 hours, before and after 6 and 9 weeks of hypercaloric diet in quiet animals submitted to a 12h light-dark cycle. To study nychtemeral cycle of SBP and HR, two periods were chosen: day (from 6.00 h to 19.00 h) and night (from 23.00 h to 6.00 h). Spontaneous baroreflex efficiency was measured using the sequence method. Spectral variability of HR and SBP was analyzed using a fast Fourier transformation on 512 consecutive values and normalized units of low (LF: 50-150 mHz, reflecting sympathetic activity) and high (HF: respiratory rate +/- 50 mHz, reflecting parasympathetic activity) frequency bands were calculated. The energy of total spectrum (from 0.004 to 1 Hz) was also studied. Body weight (12.4 +/- 0.9 vs 14.9 +/- 0.9 kg, p < 0.05). SBP (132 +/- 1 vs 147 +/- 1 mmHg, p < 0.05) significantly increased after 9 weeks of hypercaloric diet. A nycthemeral HR rhythm was present at baseline (day: 79 +/- 1 vs night: 71 +/- 1 bpm) but not after 9 weeks (day: 91 +/- 4 bpm ; night: 86 +/- 2 bpm). Concomitantly, the efficiency of spontaneous baroreflex decreased at 6 weeks (36 +/- 1 vs 42 +/- 2 mmHg/ms, p < 0.05). A significant decrease in HF energy of HRV was found after 6 but not after 9 weeks. LF energy of SBPV was increased at 6 but not at 9 weeks (table). [table: see text] In conclusion, this study shows that an hyperlipidic and hypercaloric diet induces transient variations in autonomic nervous system activity which could be the physiopathological link between obesity, insulin-resistance and arterial hypertension.

  16. Twenty-Four-Hour Real-Time Continuous Monitoring of Cerebral Edema in Rabbits Based on a Noninvasive and Noncontact System of Magnetic Induction

    Directory of Open Access Journals (Sweden)

    Gen Li

    2017-03-01

    Full Text Available Cerebral edema is a common disease, secondary to craniocerebral injury, and real-time continuous monitoring of cerebral edema is crucial for treating patients after traumatic brain injury. This work established a noninvasive and noncontact system by monitoring the magnetic induction phase shift (MIPS which is associated with brain tissue conductivity. Sixteen rabbits (experimental group n = 10, control group, n = 6 were used to perform a 24 h MIPS and intracranial pressure (ICP simultaneously monitored experimental study. For the experimental group, after the establishment of epidural freeze-induced cerebral edema models, the MIPS presented a downward trend within 24 h, with a change magnitude of −13.1121 ± 2.3953°; the ICP presented an upward trend within 24 h, with a change magnitude of 12–41 mmHg. The ICP was negatively correlated with the MIPS. In the control group, the MIPS change amplitude was −0.87795 ± 1.5146 without obvious changes; the ICP fluctuated only slightly at the initial value of 12 mmHg. MIPS had a more sensitive performance than ICP in the early stage of cerebral edema. These results showed that this system is basically capable of monitoring gradual increases in the cerebral edema solution volume. To some extent, the MIPS has the potential to reflect the ICP changes.

  17. Twenty-Four-Hour Blood Pressure Monitoring to Predict and Assess Impact of Renal Denervation: The DENERHTN Study (Renal Denervation for Hypertension).

    Science.gov (United States)

    Gosse, Philippe; Cremer, Antoine; Pereira, Helena; Bobrie, Guillaume; Chatellier, Gilles; Chamontin, Bernard; Courand, Pierre-Yves; Delsart, Pascal; Denolle, Thierry; Dourmap, Caroline; Ferrari, Emile; Girerd, Xavier; Michel Halimi, Jean; Herpin, Daniel; Lantelme, Pierre; Monge, Matthieu; Mounier-Vehier, Claire; Mourad, Jean-Jacques; Ormezzano, Olivier; Ribstein, Jean; Rossignol, Patrick; Sapoval, Marc; Vaïsse, Bernard; Zannad, Faiez; Azizi, Michel

    2017-03-01

    The DENERHTN trial (Renal Denervation for Hypertension) confirmed the blood pressure (BP) lowering efficacy of renal denervation added to a standardized stepped-care antihypertensive treatment for resistant hypertension at 6 months. We report here the effect of denervation on 24-hour BP and its variability and look for parameters that predicted the BP response. Patients with resistant hypertension were randomly assigned to denervation plus stepped-care treatment or treatment alone (control). Average and standard deviation of 24-hour, daytime, and nighttime BP and the smoothness index were calculated on recordings performed at randomization and 6 months. Responders were defined as a 6-month 24-hour systolic BP reduction ≥20 mm Hg. Analyses were performed on the per-protocol population. The significantly greater BP reduction in the denervation group was associated with a higher smoothness index (P=0.02). Variability of 24-hour, daytime, and nighttime BP did not change significantly from baseline to 6 months in both groups. The number of responders was greater in the denervation (20/44, 44.5%) than in the control group (11/53, 20.8%; P=0.01). In the discriminant analysis, baseline average nighttime systolic BP and standard deviation were significant predictors of the systolic BP response in the denervation group only, allowing adequate responder classification of 70% of the patients. Our results show that denervation lowers ambulatory BP homogeneously over 24 hours in patients with resistant hypertension and suggest that nighttime systolic BP and variability are predictors of the BP response to denervation. URL: https://www.clinicaltrials.gov. Unique identifier: NCT01570777. © 2017 American Heart Association, Inc.

  18. Twenty-four-hour Tl-201 delayed scan underestimates myocardial viability in patients with acute myocardial infarction after percutaneous transluminal coronary angioplasty

    Energy Technology Data Exchange (ETDEWEB)

    Mochizuki, Teruhito; Sugawara, Yoshifumi; Kikuchi, Takanori; Ikezoe, Junpei [Ehime Univ., Matsuyama (Japan). School of Medicine; Murase, Kenya; Higashino, Hiroshi; Miyagawa, Masao

    2001-04-01

    Myocardial viability in area at risk of acute myocardial infarction (AMI) after reperfusion therapy may be underestimated by the 24-hour images due to reverse redistribution (r-RD). Subjects were 37 AMI patients in whom Tc-99m pyrophosphate (PYP)/Tl-201 dual-isotope SPECT was positive. The 24-hour delayed scan was performed with only a Tl window. One month later, follow up rest Tl SPECT was performed to evaluate myocardial viability. In early (at PYP/Tl-201 dual-isotope SPECT), 24-hour, and one month follow up Tl studies, Tl uptake in the area of AMI was scored into four grades: 3 as normal to 0 as severely reduced. The scores were evaluated. Among the 37 AMI lesions, there were 16 r-RD, 3 RD, 16 fixed defect (FD) and 2 normal (positive PYP and normal Tl). Mean Tl scores were early; 1.4{+-}1.1, 24-hr; 0.9{+-}0.9 and one month; 1.3{+-}1.1. The 24-hour Tl score was lower than the early and one month Tl scores (p<0.01). Reverse redistribution is frequently observed in an area at risk where PYP SPECT was positive. Nuclear medicine physicians should be aware of the existence of frequent r-RD in Tl scan to avoid the underestimation of myocardial viability in the acute phase after PTCA. (author)

  19. Twenty-Four Hour Total and Dietary Fat Oxidation in Lean, Obese and Reduced-Obese Adults with and without a Bout of Exercise

    Science.gov (United States)

    Bergouignan, Audrey; Kealey, Elizabeth H.; Schmidt, Stacy L.; Jackman, Matthew R.; Bessesen, Daniel H.

    2014-01-01

    Background It has been hypothesized that obese and reduced-obese individuals have decreased oxidative capacity, which contributes to weight gain and regain. Recent data have challenged this concept. Objective To determine (1) whether total and dietary fat oxidation are decreased in obese and reduced-obese adults compared to lean but increase in response to an acute exercise bout and (2) whether regular physical activity attenuates these metabolic alterations. Design We measured 24-hr total (whole-room calorimetry) and dietary fat (14C-oleate) oxidation in Sedentary Lean (BMI = 21.5±1.6; n = 10), Sedentary Obese (BMI = 33.6±2.5; n = 9), Sedentary Reduced-Obese (RED-SED; BMI = 26.9±3.7; n = 7) and in Physically Active Reduced-Obese (RED-EX; BMI = 27.3±2.8; n = 12) men and women with or without an acute exercise bout where energy expended during exercise was not replaced. Results Although Red-SED and Red-EX had a similar level of fatness, aerobic capacity and metabolic profiles were better in Red-EX only compared to Obese subjects. No significant between-group differences were seen in 24-hr respiratory quotient (RQ, Lean: 0.831±0.044, Obese: 0.852±0.023, Red-SED: 0.864±0.037, Red-EX: 0.842±0.039), total and dietary fat oxidation. A single bout of exercise increased total (+27.8%, p<0.0001) and dietary (+6.6%, p = 0.048) fat oxidation across groups. Although exercise did not impact RQ during the day, it decreased RQ during sleep (p = 0.01) in all groups. Red-EX oxidized more fat overnight than Red-SED subjects under both resting (p = 0.036) and negative energy balance (p = 0.003) conditions, even after adjustment for fat-free mass. Conclusion Obese and reduced-obese individuals oxidize as much fat as lean both under eucaloric and negative energy balance conditions, which does not support the hypothesis of reduced oxidative capacity in these groups. Reduced-obese individuals who exercise regularly have markers of metabolic health similar to those seen in lean adults. Both the acute and chronic effects of exercise were primarily observed at night suggesting an important role of sleep in the regulation of lipid metabolism. PMID:24714529

  20. Twenty-four hour total and dietary fat oxidation in lean, obese and reduced-obese adults with and without a bout of exercise.

    Directory of Open Access Journals (Sweden)

    Audrey Bergouignan

    Full Text Available It has been hypothesized that obese and reduced-obese individuals have decreased oxidative capacity, which contributes to weight gain and regain. Recent data have challenged this concept.To determine (1 whether total and dietary fat oxidation are decreased in obese and reduced-obese adults compared to lean but increase in response to an acute exercise bout and (2 whether regular physical activity attenuates these metabolic alterations.We measured 24-hr total (whole-room calorimetry and dietary fat (14C-oleate oxidation in Sedentary Lean (BMI = 21.5±1.6; n = 10, Sedentary Obese (BMI = 33.6±2.5; n = 9, Sedentary Reduced-Obese (RED-SED; BMI = 26.9±3.7; n = 7 and in Physically Active Reduced-Obese (RED-EX; BMI = 27.3±2.8; n = 12 men and women with or without an acute exercise bout where energy expended during exercise was not replaced.Although Red-SED and Red-EX had a similar level of fatness, aerobic capacity and metabolic profiles were better in Red-EX only compared to Obese subjects. No significant between-group differences were seen in 24-hr respiratory quotient (RQ, Lean: 0.831±0.044, Obese: 0.852±0.023, Red-SED: 0.864±0.037, Red-EX: 0.842±0.039, total and dietary fat oxidation. A single bout of exercise increased total (+27.8%, p<0.0001 and dietary (+6.6%, p = 0.048 fat oxidation across groups. Although exercise did not impact RQ during the day, it decreased RQ during sleep (p = 0.01 in all groups. Red-EX oxidized more fat overnight than Red-SED subjects under both resting (p = 0.036 and negative energy balance (p = 0.003 conditions, even after adjustment for fat-free mass.Obese and reduced-obese individuals oxidize as much fat as lean both under eucaloric and negative energy balance conditions, which does not support the hypothesis of reduced oxidative capacity in these groups. Reduced-obese individuals who exercise regularly have markers of metabolic health similar to those seen in lean adults. Both the acute and chronic effects of exercise were primarily observed at night suggesting an important role of sleep in the regulation of lipid metabolism.

  1. Twenty-four-hour simultaneous subcutaneous basal-bolus administration of insulin and amylin in adolescents with type 1 diabetes decreases postprandial hyperglycemia

    Science.gov (United States)

    The purpose of this study was to examine the effect of continuous subcutaneous (sc) replacement of amylin and insulin for a 24-h period on glucose homeostasis in adolescents with type 1 diabetes. Thirteen adolescents with type 1 diabetes on insulin pump therapy participated in a randomized, controll...

  2. Twenty-four hours, or five days, of continuous sleep deprivation or experimental sleep fragmentation do not alter thirst or motivation for water reward in rats.

    Science.gov (United States)

    Christie, Michael A; McCarley, Robert W; Strecker, Robert E

    2010-12-25

    Sleep disruption results in an increased demand for energy, which typically causes hyperphagia in an attempt to redress the energy metabolism imbalance. Therefore, experiments combining food reward and sleep disruption may underestimate the effect of sleep disruption due to their contradictory influences on behavior (for example on operant measures of attention). In contrast, water is not a central component of energy metabolism and thus thirst may not be affected by sleep disruption. However, little work has been done examining the effect of sleep disruption on thirst and motivation for water. The effect of total sleep deprivation (SD) and experimental sleep fragmentation (SF) on thirst and motivation for water was assessed. In experiment 1 (using 22 month old male Fisher-Norway rats) the amount of water consumed during a 15 min period immediately following a period of 24h SD or SF (in which water was not available) was measured, and, in a separate session, the amount of water consumed during the 24h of SD or SF was measured. Thereafter, the effect of 5 days SD or SF on motivation for water was assessed with the progressive ratio task (using water reward), which is widely used to assess motivation. Experiment 2 (using 6 month, and 22 month, old male Sprague- Dawley rats) followed an identical design except that the SF condition was dropped (due to a lack of any difference between the SD and SF conditions in experiment 1), and only the 6 month old rats experienced the full 5 day SD condition. Daily measurements of body weight and food consumption were recorded in experiment 2 in order to confirm previously published findings that food consumption goes up and body weight declines in sleep deprived rats. In both experiments the quantity of water rats consumed during a 15 min period immediately following the 24h period of sleep disruption, or consumed during the 24h period of SD or SF, did not change compared to control rats. Furthermore, 5 days of SD or SF had no effect on breakpoint in the progressive ratio task indicating that 5 days of SD or SF did not alter motivation for water reward. As previously reported, food consumption increased and body weight decreased during the 5 days of SD. in experiment 2. The findings indicate that although sleep disruption increases food consumption and decreases body weight, it does not alter thirst or motivation for water reward. Thus, water restriction is well suited for experiments examining the effect of sleep disruption on reward motivated behavioral tests in rats. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  3. The acute effects of twenty-four hours of sleep loss on the performance of national-caliber male collegiate weightlifters.

    Science.gov (United States)

    Blumert, Peter A; Crum, Aaron J; Ernsting, Mark; Volek, Jeff S; Hollander, Daniel B; Haff, Erin E; Haff, G Gregory

    2007-11-01

    Currently, the degree to which sleep loss influences weightlifting performance is unknown. This study compared the effects of 24 hours of sleep loss on weightlifting performance and subjective ratings of psychological states pre-exercise and postexercise in national-caliber male collegiate weightlifters. Nine males performed a maximal weightlifting protocol following 24 hours of sleep loss and a night of normal sleep. The subjects participated in a randomized, counterbalanced design with each sleep condition separated by 7 days. Testosterone and cortisol levels were quantified prior to, immediately after, and 1 hour after the resistance training session. Additionally, profile of mood states and subjective sleepiness were evaluated at the same time points. The resistance training protocol consisted of several sets of snatches, clean and jerks, and front squats. Performance was evaluated as individual exercise volume load, training intensity and overall workout volume load, and training intensity. During each training session the maximum weight lifted for the snatch, clean and jerk, and front squat were noted. No significant differences were found for any of the performance variables. A significant decrease following the sleep condition was noted for cortisol concentration immediately after and 1 hour postexercise. Vigor, fatigue, confusion, total mood disturbance, and sleepiness were all significantly altered by sleep loss. These data suggest that 24 hours of sleep loss has no adverse effects on weightlifting performance. If an athlete is in an acute period of sleep loss, as noticed by negative mood disturbances, it may be more beneficial to focus on the psychological (motivation) rather than the physiological aspect of the sport.

  4. Twenty-four-hour changes of S-adenosylmethionine, S-adenosylhomocysteine adenosine and their metabolizing enzymes in rat liver; possible physiological significance in phospholipid methylation.

    Science.gov (United States)

    Chagoya de Sánchez, V; Hernández-Muñoz, R; Sánchez, L; Vidrio, S; Yáñez, L; Suárez, J

    1991-01-01

    1. The metabolic control of adenosine concentration in the rat liver through the 24-hr cycle is related to the activity of adenosine-metabolizing enzymes [5'-nucleotidase (5'N), adenosine deaminase (A.D.), adenosine kinase (A.K.) and S-adenosylhomocysteine hydrolase (SAH-H)]. 2. Two peaks of adenosine were observed, one at 12:00 hr caused by high activity of 5'N and SAH-H, and the other at 02:00 hr, caused by a decrease in purine catabolism and purine utilization, low activity of SAH-H and de novo purine formation. 3. The similarity of the adenosine and S-adenosylmethionine (SAM) profiles through the 24-hr cycle suggests a role of adenosine in transmethylation reactions, because, during the night (02:00 hr), the metabolic conditions favor the formation and accumulation of S-adenosylhomocysteine (SAH), with consequent inhibition of transmethylation reactions. 4. In the 24-hr variation of phosphatidylcholine (PC) and phosphatidylethanolamine (PE), the lowest ratio of PC/PE was observed at 24:00-02:00 hr when SAH concentration is high, whereas the highest PC/PE ratio occurs at the same time as one of the SAM/SAH ratio maxima.

  5. Twenty-four-hour central blood pressure is not better associated with hypertensive target organ damage than 24-h peripheral blood pressure.

    Science.gov (United States)

    de la Sierra, Alejandro; Pareja, Julia; Fernández-Llama, Patricia; Armario, Pedro; Yun, Sergi; Acosta, Eva; Calero, Francesca; Vázquez, Susana; Blanch, Pedro; Sierra, Cristina; Oliveras, Anna

    2017-10-01

    Central blood pressure (BP) is increasingly considered as a better estimator of hypertension associated risks. We aimed to evaluate the association of 24-h central BP, in comparison with 24-h peripheral BP, with the presence of target organ damage (TOD). Cross-sectional study of 208 hypertensive patients, aged 57 ± 12 years, 34% women. Office (mean of 4 measurements) and 24-h central and peripheral BP were measured by the oscillometric Mobil-O-Graph device. TOD was assessed at cardiac (left ventricular hypertrophy by echocardiography), renal (reduction of glomerular filtration rate and/or microalbuminuria), and arterial (increased aortic pulse wave velocity) levels. A total of 107 patients (51.4%) had TOD (77, 35% patients left ventricular hypertrophy; 54, 25.9% renal abnormalities; and 40, 19.2% arterial stiffness). All SBP and pulse BP estimates (office, 24-h, daytime, and night-time) were associated with the presence of TOD, after adjustment for age, sex, and antihypertensive treatment, with higher odds ratios for ambulatory-derived values. Odds ratios for central and peripheral BP were similar for all office, 24-h, daytime, and night-time BP. After simultaneous adjustment, peripheral, but not central, 24-h and night-time SBP and pulse pressures were associated with the presence of TOD. TOD in hypertension is associated with BP elevation, independently of the type of measurement (office or ambulatory, central or peripheral). Central BP, even monitored during 24 h, is not better associated with TOD than peripheral BP. These results do not support a routine measurement of 24-h central BP.

  6. Twenty four hour insulin infusion impairs the ability of plasma from healthy subjects and Type 2 diabetic patients to promote cellular cholesterol efflux

    NARCIS (Netherlands)

    Dullaart, RPF; van Tol, A

    Removal of cholesterol from peripheral cells by high density lipoproteins (HDL) is regarded as an important defence mechanism against atherosclerosis development. PLTP is involved in the generation of pre beta -HDL that can act as initial accepters of cellular cholesterol. Exogenous

  7. Twenty-four Hour Endocrine and Metabolic Profiles Following Consumption of High Fructose Corn Syrup-, Sucrose- Fructose-, and Glucose-Sweetened Beverages with Meals

    Science.gov (United States)

    We have reported that compared with glucose-sweetened beverages, consuming fructose-sweetened beverages with meals results in lower 24-h circulating glucose, insulin and leptin concentrations, and elevated triacylglycerol (TG). However, pure fructose and glucose are not commonly used as sweeteners. ...

  8. Diurnal Variation and Twenty-Four Hour Sleep Deprivation Do Not Alter Supine Heart Rate Variability in Healthy Male Young Adults

    Science.gov (United States)

    Elvsåshagen, Torbjørn; Zak, Nathalia; Norbom, Linn B.; Pedersen, Per Ø.; Quraishi, Sophia H.; Bjørnerud, Atle; Malt, Ulrik F.; Groote, Inge R.; Kaufmann, Tobias; Andreassen, Ole A.; Westlye, Lars T.

    2017-01-01

    Heart rate variability (HRV) has become an increasingly popular index of cardiac autonomic control in the biobehavioral sciences due to its relationship with mental illness and cognitive traits. However, the intraindividual stability of HRV in response to sleep and diurnal disturbances, which are commonly reported in mental illness, and its relationship with executive function are not well understood. Here, in 40 healthy adult males we calculated high frequency HRV—an index of parasympathetic nervous system (PNS) activity—using pulse oximetry during brain imaging, and assessed attentional and executive function performance in a subsequent behavioral test session at three time points: morning, evening, and the following morning. Twenty participants were randomly selected for total sleep deprivation whereas the other 20 participants slept as normal. Sleep deprivation and morning-to-night variation did not influence high frequency HRV at either a group or individual level; however, sleep deprivation abolished the relationship between orienting attention performance and HRV. We conclude that a day of wake and a night of laboratory-induced sleep deprivation do not alter supine high frequency HRV in young healthy male adults. PMID:28151944

  9. A follow-up urine sample has limited value after treatment for urinary tract infection in children

    DEFF Research Database (Denmark)

    Lytzen, Rebekka; Kaalund-Jørgensen, Kristine; Ahmed, Akhlaq;

    2015-01-01

    INTRODUCTION: A routine follow-up urine sample (FUS) in the form of a midstream urine sample (MSU) is recommended after treatment for urinary tract infection (UTI) according to the Danish Paediatric Society (DPS) and "Lægehåndbogen" published by Danish Regions. We studied the effect of FUS...... with a focus on patients without symptoms at the time of FUS. METHODS: Consecutive patients below 16.0 years treated for upper or lower UTI from 1 January 2009 to 31 December 2009 at Hvidovre Hospital in accordance with the guidelines of the department and the DPS. All patients were asked to provide a FUS...... within 21 days. RESULTS: A total of 87 patients were treated for upper UTI: 59 girls and 28 boys, the median age was 1.1 year (range: 0.1-15.6 years); and 42 girls were treated for lower UTI, their median age was 8.2 years (range: 2.5-15.3 years). After treatment, the risk of a UTI was 0% (0/87) after...

  10. A comparative study of bacterial isolates from the urine samples of AIDS and non-AIDS patients in Benue, Nigeria

    Institute of Scientific and Technical Information of China (English)

    Okwori EE; Nwadioha SI; Jombo GTA; Nwokedi EOP; Odimayo MS

    2010-01-01

    Objective:To determine the common bacterial causes of urinary tract infection and their antibiotic susceptibility pattern in AIDS patients versus non-AIDS patients. Methods: One thousand consecutive AIDS patients with signs and symptoms of AIDS and non-AIDS patients (served as control) each on admission were recruited into the study between January 2005 to January 2008, in Federal Medical Center, Makurdi. Urine samples were collected with sterile universal bottles and analysed with appropriate laboratory methods and antibiotic susceptibility test was carried out by disk diffusion technique in accordance with National Committee for Clinical Laboratory Standards (NCCLS, now CLSI) criteria. The results were analysed using SPSS 11.0 statistical software. Results:Urine samples of AIDS patients with urinary infection had a more spectrum of micro-organisms including Candida organisms, Pseudomonas aeruginosa and Staphylococcus aureus. Ceftriaxone, Ceftazidime or Ciprofloxacin had a remarkably high anti-bacterial activity across the two study groups. A general resistance was recorded in ampicillin, tetracycline and co-trimoxazole. There was no significant difference in antibiotic susceptibility patterns between AIDS and non-AIDS patients(P>0.05). Conclusions:A reduction in unnecessary use of antibiotics as well as infection control should be encouraged in our health facilities.

  11. Rapid detection of extended-spectrum-β-lactamase-producing enterobacteriaceae from urine samples by use of the ESBL NDP test.

    Science.gov (United States)

    Dortet, Laurent; Poirel, Laurent; Nordmann, Patrice

    2014-10-01

    From June to September 2012, 500 urine samples were recovered from patients with urinary tract infections (UTI) due to Gram-negative bacilli (≥ 10(4) leukocytes/ml and ≥ 10(5) Gram-negative isolates/ml) who visited the University hospital Bicêtre (France). They were challenged with extended-spectrum-β-lactamase (ESBL)-producing Enterobacteriaceae (ESBL-E) using the rapid diagnostic ESBL NDP test. Results of the ESBL NDP test were compared to the results of the double-disc susceptibility test (DDST) performed on solid-agar plates and molecular identification of the β-lactamase genes. Among the 450 nonduplicate urine samples, 11.3% were positive for ESBL-E by using the DDST, the ESBL determinants being mostly of the CTX-M type (CTX-M-15) according to molecular testing. Results of the ESBL NDP test were obtained within 15 min. The sensitivity and specificity of the ESBL NDP test were 98% and 99.8%, respectively, whereas the positive and negative predictive values of this test were 98% and 99.8%, respectively. A perfect correlation between cefotaxime resistance and positivity of the ESBL NDP test was observed. Therefore, the ESBL NDP test offers a powerful tool for a rapid identification of ESBL-E and associated resistance to expanded-spectrum cephalosporins. It may be useful in particular for guiding first-line antibiotic therapy.

  12. Urine-sample-derived human induced pluripotent stem cells as a model to study PCSK9-mediated autosomal dominant hypercholesterolemia.

    Science.gov (United States)

    Si-Tayeb, Karim; Idriss, Salam; Champon, Benoite; Caillaud, Amandine; Pichelin, Matthieu; Arnaud, Lucie; Lemarchand, Patricia; Le May, Cédric; Zibara, Kazem; Cariou, Bertrand

    2016-01-01

    Proprotein convertase subtilisin kexin type 9 (PCSK9) is a critical modulator of cholesterol homeostasis. Whereas PCSK9 gain-of-function (GOF) mutations are associated with autosomal dominant hypercholesterolemia (ADH) and premature atherosclerosis, PCSK9 loss-of-function (LOF) mutations have a cardio-protective effect and in some cases can lead to familial hypobetalipoproteinemia (FHBL). However, limitations of the currently available cellular models preclude deciphering the consequences of PCSK9 mutation further. We aimed to validate urine-sample-derived human induced pluripotent stem cells (UhiPSCs) as an appropriate tool to model PCSK9-mediated ADH and FHBL. To achieve our goal, urine-sample-derived somatic cells were reprogrammed into hiPSCs by using episomal vectors. UhiPSC were efficiently differentiated into hepatocyte-like cells (HLCs). Compared to control cells, cells originally derived from an individual with ADH (HLC-S127R) secreted less PCSK9 in the media (-38.5%; P=0.038) and had a 71% decrease (Pcells originally derived from an individual with FHBL (HLC-R104C/V114A) displayed a strong decrease in PCSK9 secretion (-89.7%; Pcells for reprogramming and hepatocyte differentiation, but also a powerful tool to further decipher PCSK9 mutations and function.

  13. Detection of N{sup 6}-methyladenosine in urine samples by electrochemiluminescence using a heated ITO electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lin Zhenyu [Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350002 (China); Wang Wanzong [Department of Orthopedics, Fuzhou General Hospital of Nanjing Military Command, Fuzhou 350025 (China); Jiang Yingyan; Qiu Bin [Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350002 (China); Chen Guonan, E-mail: gnchen@fzu.edu.c [Ministry of Education Key Laboratory of Analysis and Detection for Food Safety, Fujian Provincial Key Laboratory of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350002 (China)

    2010-12-30

    A sensitive and rapid electrochemiluminescence (ECL) method for the detection of N{sup 6}-Methyladenosine (m6A) in urine samples on a heated indium-tin-oxide (ITO) electrode is presented. The ECL intensity of Tris(2,2'-bipyridyl) dichlororuthenium(II)hexahydrate (Ru(bpy){sub 3}{sup 2+}) can be enhanced by the presence of m6A. Experimental results showed that the change of ECL intensities ({Delta}I) of the Ru(bpy){sub 3}{sup 2+} between before and after addition of m6A was affected by the working electrode surface temperature (T{sub e}); the highest {Delta}I occurred at 31 {sup o}C. Under optimum conditions, the {Delta}I had a linear relationship with the m6A concentration in the range of 1.9 x 10{sup -9}-3.9 x 10{sup -6} mol/L and a detection limit of 7.7 x 10{sup -10} mol/L (S/N = 3) at T{sub e} = 31 {sup o}C. The recovery of m6A standards added to urine samples verified the accuracy of the proposed method.

  14. Assessment of DDT, DDE, and 1-hydroxypyrene levels in blood and urine samples in children from Chiapas Mexico.

    Science.gov (United States)

    Martínez-salinas, Rebeca I; Pérez-Maldonado, Iván N; Batres-Esquivel, Lilia E; Flores-Ramírez, Rogelio; Díaz-Barriga, Fernando

    2011-08-01

    The aim of this study was assess co-exposure to DDT, DDE (main DDT metabolite), and PAHs (1-hydroxypyrene) in areas where biomass is used to cook and to heat homes and where DDT was used to combat malaria transmission. During 2009, we analyzed a total of 190 blood and urine samples from children living in six communities in Mexico. Quantitative analyses of DDT and DDE were performed using gas chromatography coupled with mass spectrometry. Analyses of 1-hydroxypyrene were performed by HPLC using a fluorescence detector. In this work, we found high levels of DDT and its principal metabolite (DDE) in the blood of children living in four communities in Chiapas located in the southeastern region of Mexico (range, urine samples (range, 0.02 to 4.82 μmol/mol creatinine). An important finding was that around one third of the children studied in these areas were co-exposed to the three compounds. This study demonstrates that children in these communities were exposed to DDT and its metabolites, and to other contaminants generated by the combustion of firewood. Therefore, the complex mixture studied in this study (PAHs and DDT/DDE) requires further research.

  15. Chiral liquid chromatography-mass spectrometry (LC-MS/MS) method development for the detection of salbutamol in urine samples.

    Science.gov (United States)

    Chan, Sue Hay; Lee, Warren; Asmawi, Mohd Zaini; Tan, Soo Choon

    2016-07-01

    A sequential solid-phase extraction (SPE) method was developed and validated using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) for the detection and quantification of salbutamol enantiomers in porcine urine. Porcine urine samples were hydrolysed with β-glucuronidase/arylsulfatase from Helix pomatia and then subjected to a double solid-phase extraction (SPE) first using the Abs-Elut Nexus SPE and then followed by the Bond Elut Phenylboronic Acid (PBA) SPE. The salbutamol enantiomers were separated using the Astec CHIROBIOTIC™ T HPLC column (3.0mm×100mm; 5μm) maintained at 15°C with a 15min isocratic run at a flow rate of 0.4mL/min. The mobile phase constituted of 5mM ammonium formate in methanol. Salbutamol and salbutamol-tert-butyl-d9 (internal standard, IS) was monitored and quantified with the multiple reaction monitoring (MRM) mode. The method showed good linearity for the range of 0.1-10ng/mL with limit of quantification at 0.3ng/mL. Analysis of the QC samples showed intra- and inter-assay precisions to be less than 5.04%, and recovery ranging from 83.82 to 102.33%.

  16. Two-phase and three-phase liquid-phase microextraction of hydrochlorothiazide and triamterene in urine samples.

    Science.gov (United States)

    Ahmad Panahi, Homayon; Ejlali, Maryam; Chabouk, Monireh

    2016-07-01

    This paper reports the applicability of two-phase and three-phase hollow fiber based liquid-phase microextraction (HF-LPME) for the extraction of hydrochlorothiazide (HYD) and triamterene (TRM) from human urine. The HYD in two-phase HF-LPME is extracted from 24 mL of the aqueous sample into an organic phase with microliter volume located inside the pores and lumen of a polypropylene hollow fiber as acceptor phase, but the TRM in three-phase HF-LPME is extracted from aqueous donor phase to organic phase and then back-extracted to the aqueous acceptor phase, which can be directly injected into HPLC for analysis. Under optimized conditions preconcentration factors of HYD and TRM were obtained as 128 and 239, respectively. The calibration curves were linear (R(2)  ≥ 0.995) in the concentration range of 1.0-100 µg/L for HYD and 2.0-100 µg/L for TRM. The limits of detection for HYD and TRM were 0.5 µg/L. The intra-day and inter-day RSD based on four replicates were obtained as ≤5.8 and ≤9.3%, respectively. The methods were successfully applied for determining the concentration of the drugs in urine samples. Copyright © 2015 John Wiley & Sons, Ltd.

  17. In-sample derivatization-solid-phase microextraction of amphetamines and ecstasy related stimulants from water and urine.

    Science.gov (United States)

    Racamonde, Inés; Rodil, Rosario; Quintana, José Benito; Cela, Rafael

    2013-04-03

    A solid-phase microextraction (SPME) method for the determination of five amphetamine type stimulants (ATSs) in water and urine samples is presented. Analytes were simultaneously derivatized with iso-butyl chloroformate (iBCF) in the aqueous sample while being extracted, improving in this way the extractability of ATSs and permitting their determination by gas chromatography-mass spectrometry (GC-MS). The SPME procedure was carefully optimized in order to achieve adequate limits of detection (LODs) for environmental concentrations. Hence, different operational parameters were considered: type of SPME coating, ionic strength, basic catalyzer and derivatizing agent amount, extraction time and temperature. The final SPME procedure consists into the extraction of 100mL of sample containing 2 g of dipotassium monohydrogen phosphate trihydrate and 100 μL of iBCF (1:1 in acetonitrile), for 40 min at 60°C with a polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber. Under these conditions, LODs in wastewater ranged from 0.4 to 2 ng L(-1), relative recoveries in the 84-114% range and relative standard deviations (RSD) lower than 15% were obtained. The application of the method to wastewater and river water samples showed the ecstasy ATS, 3,4-methylenedioxymethamphetamine (MDMA), as the most frequently detected, followed by methamphetamine, in concentrations around 20 ng L(-1). Finally, the method was downscaled and also validated with urine samples, proving its good performance with this matrix too: RSD<11%, recoveries in the 98-110% range and LODs lower than 0.1 μg L(-1).

  18. Simultaneous Separation of Eight Benzodiazepines in Human Urine Using Field-Amplified Sample Stacking Micellar Electrokinetic Chromatography.

    Science.gov (United States)

    Oledzka, Ilona; Kulińska, Zofia; Prahl, Adam; Baczek, Tomasz

    2015-01-01

    A novel approach for the simultaneous quantification of eight benzodiazepines (BZDs) using dispersive liquid-liquid microextraction (DLLME) and field-amplified sample stacking (FASS) combined with micellar electrokinetic chromatography (MEKC) was investigated and evaluated in the context of precision, accuracy, sensitivity, linearity, detection and limits of quantification (LOQ). The absolute recovery rates of BZDs were above 90.65%. The limits of detection (LOD) were 20 ng/mL for chlordiazepoxide, estazolam, temazepam and midazolam, and 30 ng/mL for clonazepam, lorazepam, lormetazepam and medazepam, while the LOQ was set at 50 ng/mL for chlordiazepoxide, estazolam, temazepam and midazolam, and 100 ng/mL for clonazepam, lorazepam, lormetazepam and medazepam. Linearity was confirmed in the range of 50-2,000 ng/mL for chlordiazepoxide, estazolam, temazepam and midazolam, and 100-2,000 ng/mL for clonazepam, lorazepam, lormetazepam and medazepam, with a correlation coefficient greater than 0.9987 for all analytes. The elaborated procedure meets all the requirements of analytical methods. During the extraction procedure, a mixture of 1 mL of ethanol and 500 µL of dichloromethane, used as the disperser and extraction solvent, respectively, was rapidly injected into 3 mL of a urine sample. A significant improvement in sensitivity was achieved when DLLME was used to extract BZDs from the urine sample and FASS as an on-line preconcentration technique was developed. For the best separation of analytes, the running buffer was composed of 30 mM SDS, 10 mM sodium tetraborate and 15% methanol (pH 8.8), whereas a sample buffer was composed of 10 mM SDS and 2 mM sodium tetraborate. Moreover, a fused-silica capillary [inner diameter (i.d.) of 75 µm and length of 50 cm], photodiode array detection, pneumatic injection for 15 s and a voltage of 23 kV were applied. The applicability of the method has been confirmed for the analysis of BZD in urine samples collected from patients who

  19. [Quantitative and qualitative bacteriological studies on urine specimens obtained by suprapubic needle aspiration and on midstream-voided samples].

    Science.gov (United States)

    Augustin, R; Seybold, G; Witzenhausen, R; Hessler, M; Niemeyer, G

    1978-06-24

    In 398 patients with suspected urinary tract infection, quantitative and qualitative bacteriological studies were conducted in urine samples obtained by suprapubic needle aspiration of the bladder (BPU) and in midstream-voided specimens (MSU) collected immediately following the aspirations. In MSU, bacteria were found in 96.5% of all cases and in BPU in only 38.2%. Of the infected MSU, 63.3% showed mixed infections, while mixed cultures were found in only 11.2% of infected BPU. In 80% of the investigated patients, the MSU contained at least one more type of bacteria than the BPU, thus indicating urethral contamination. Of the patients with bladder bacteriuria, only 74% had bacterial counts of 10(5)/ml or more in the midstream-voided urine. Accordingly, 26% of the urinary tract infections diagnosed by bladder aspiration would not have been recognized on the basis of a single bacterial count in the midstream-voided urine. On the other hand, about 4% of patients with bacterial counts of 10(5)/ml or more in the MSU had a sterile bladder aspirate. In 72.4% of the infected BPU, E. coli was found, followed in frequency by Enterococcus (14.5%). In the infected MSU, however, Enterococcus was more frequent than C. coli (65.6% and 61.7% respectively). Thus, E. coli appears to be the most important etiological species in infections of the bladder and the kidneys, while Enterococcus seems to be the most frequent contaminant during urethral passage. The most frequent bacterial combination in mixed cultures in both BPU and MSU was that of E. coli and Enterococcus.

  20. Phase I metabolism of the highly potent synthetic cannabinoid MDMB-CHMICA and detection in human urine samples.

    Science.gov (United States)

    Franz, Florian; Angerer, Verena; Moosmann, Bjoern; Auwärter, Volker

    2017-05-01

    Among the recently emerged synthetic cannabinoids, MDMB-CHMICA (methyl N-{[1-(cyclohexylmethyl)-1H-indol-3-yl]carbonyl}-3-methylvalinate) shows an extraordinarily high prevalence in intoxication cases, necessitating analytical methods capable of detecting drug uptake. In this study, the in vivo phase I metabolism of MDMB-CHMICA was investigated using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) and liquid chromatography-electrospray ionization-quadrupole time-of-flight-mass spectrometry (LC-ESI-Q ToF-MS) techniques. The main metabolites are formed by hydrolysis of the methyl ester and oxidation of the cyclohexyl methyl side chain. One monohydroxylated metabolite, the ester hydrolysis product and two further hydroxylated metabolites of the ester hydrolysis product are suggested as suitable targets for a selective and sensitive detection in urine. All detected in vivo metabolites could be verified in vitro using a human liver microsome assay. Two of the postulated main metabolites were successfully included in a comprehensive LC-ESI-MS/MS screening method for synthetic cannabinoid metabolites. The screening of 5717 authentic urine samples resulted in 818 cases of confirmed MDMB-CHMICA consumption (14%). Since the most common route of administration is smoking, smoke condensates were analyzed to identify relevant thermal degradation products. Pyrolytic cleavage of the methyl ester and amide bond led to degradation products which were also formed metabolically. This is particularly important in hair analysis, where detection of metabolites is commonly considered a proof of consumption. In addition, intrinsic activity of MDMB-CHMICA at the CB1 receptor was determined applying a cAMP accumulation assay and showed that the compound is a potent full agonist. Based on the collected data, an enhanced interpretation of analytical findings in urine and hair is facilitated. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John

  1. Activity-Based Detection of Consumption of Synthetic Cannabinoids in Authentic Urine Samples Using a Stable Cannabinoid Reporter System.

    Science.gov (United States)

    Cannaert, Annelies; Franz, Florian; Auwärter, Volker; Stove, Christophe P

    2017-09-05

    Synthetic cannabinoids (SCs) continue to be the largest group of new psychoactive substances (NPS) monitored by the European Monitoring Center of Drugs and Drugs of Abuse (EMCDDA). The identification and subsequent prohibition of single SCs has driven clandestine chemists to produce analogues of increasing structural diversity, intended to evade legislation. That structural diversity, combined with the mostly unknown metabolic profiles of these new SCs, poses a big challenge for the conventional targeted analytical assays, as it is difficult to screen for "unknown" compounds. Therefore, an alternative screening method, not directly based on the structure but on the activity of the SC, may offer a solution for this problem. We generated stable CB1 and CB2 receptor activation assays based on functional complementation of a split NanoLuc luciferase and used these to test an expanded set of recent SCs (UR-144, XLR-11, and their thermal degradation products; AB-CHMINACA and ADB-CHMINACA) and their major phase I metabolites. By doing so, we demonstrate that several major metabolites of these SCs retain their activity at the cannabinoid receptors. These active metabolites may prolong the parent compound's psychotropic and physiological effects and may contribute to the toxicity profile. Utility of the generated stable cell systems as a first-line screening tool for SCs in urine was also demonstrated using a relatively large set of authentic urine samples. Our data indicate that the stable CB reporter assays detect CB receptor activation by extracts of urine in which SCs (or their metabolites) are present at low- or subnanomolar (ng/mL) level. Hence, the developed assays do not only allow activity profiling of SCs and their metabolites, it may also serve as a screening tool, complementing targeted and untargeted analytical assays and preceding analytical (mass spectrometry based) confirmation.

  2. Bilirubin - urine

    Science.gov (United States)

    Conjugated bilirubin - urine; Direct bilirubin - urine ... Bilirubin is not normally found in the urine. ... Increased levels of bilirubin in the urine may be due to: Biliary tract disease Cirrhosis Gallstones in the biliary tract Hepatitis Liver disease ...

  3. The multi-concentration and two-dimensional capillary electrophoresis method for the analysis of drugs in urine samples

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A novel method has been developed by integration of multi-concentration and two-dimensional(2D) capillary electrophoresis(CE) for simultaneous enhancement of detection sensitivity and separation power in complex samples.Capillary zone electrophoresis(CZE) was used as the first dimension separation according to mobilities,from which the effluent fractions were further analyzed by micellar electrokinetic capillary chromatography(MEKC) acting as the second dimension.Cation-selective exhaustive injection(CSEI) preconcentration method was used to introduce more analytes into the capillary.Furthermore,pH junction and sweeping dual concentration strategies were employed to avoid sample zone diffusion at the interface.The resulting electrophoregram was quite different from that of either CZE or MEKC separation.Up to(0.5-1.2) ×104 fold improvements in sensitivity were obtained relative to the conventional electrokinetic injection method.The proposed method was successfully applied to the determination of drugs in human urine.

  4. Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

    Science.gov (United States)

    Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

    2011-01-01

    To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

  5. Validation of a high performance liquid chromatography analysis for the determination of noradrenaline and adrenaline in human urine with an on-line sample purification

    DEFF Research Database (Denmark)

    Hansen, Åse Marie; Kristiansen, J; Nielsen, J L

    1999-01-01

    A high performance liquid chromatography (HPLC) method with fluorescence detection including an on-line purification was established for determination of catecholamines in human urine. The method was evaluated using samples of pooled urine spiked with catecholamines and validated for measurements...... deviation of the method was sufficiently low to distinguish between persons working with two different processes of garbage collection, i.e. collection using four wheeled containers versus collection using bins....

  6. Highly specific quantification of ergotamine in urine, blood, and hair samples by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Favretto, Donata; Frison, Giampietro; Vogliardi, Susanna; Ferrara, Santo Davide

    2007-06-01

    Ergotamine has been used for therapeutic purposes since the 1950s, usually to treat vascular headache. It is highly toxic and in large, repeated doses can produce all the symptoms of ergot poisoning. A selective and sensitive method, based on liquid chromatography-tandem mass spectrometry (LC-MS2), has been developed for quantifying ergotamine in biological fluids with use of a quick and easy sample preparation. Ergotamine and the internal standard, trideuterated lysergic acid diethylamide, were extracted from human urine, blood, and hair by means of liquid-liquid extraction at alkaline pH. Gradient elution on a cyanopropyl column was used for chromatographic separation. Positive ion electrospray ionization and tandem mass spectrometry determination by collision-induced dissociation were performed in an ion trap mass spectrometer. The method was validated and successfully applied to a case of iatrogenic ergotism resulting from the intake of ergotamine tartrate for treating headache. For the first time, ergotamine was identified and quantified in hair. The ergotamine concentrations measured were 320 pg/mL in blood, 100 pg/mL in urine, 24 pg/mg in proximal hair, and 15 pg/mg in distal hair.

  7. Rapid and sensitive detection of fluoroquinolone-resistant Escherichia coli from urine samples using a genotyping DNA microarray.

    Science.gov (United States)

    Yu, Xiaolei; Susa, Milorad; Weile, Jan; Knabbe, Cornelius; Schmid, Rolf D; Bachmann, Till T

    2007-10-01

    Urinary tract infections (UTI) are among the most common bacterial infections in humans, with Escherichia coli being the major cause of infection. Fluoroquinolone resistance of uropathogenic E. coli has increased significantly over the last decade. In this study a microarray-based assay was developed and applied, which provides a rapid, sensitive and specific detection of fluoroquinolone-resistant E. coli in urine. The capture probes were designed against previously identified and described hotspots for quinolone resistance (codons 83 and 87 of gyrA). The key goals of this development were to reduce assay time while increasing the sensitivity and specificity as compared with a pilot version of a gyrA genotyping DNA microarray. The performance of the assay was demonstrated with pure cultures of 30 E. coli isolates as well as with urine samples spiked with 6 E. coli isolates. The microarray results were confirmed by standard DNA sequencing and were in full agreement with the phenotypic antimicrobial susceptibility testing using standard methods. The DNA microarray test displayed an assay time of 3.5h, a sensitivity of 100CFU/ml, and the ability to detect fluoroquinolone-resistant E. coli in the presence of a 10-fold excess of fluoroquinolone-susceptible E. coli cells. As a consequence, we believe that this microarray-based determination of antibiotics resistance has a true potential for the application in clinical routine laboratories in the future.

  8. Four-way calibration applied to the simultaneous determination of folic acid and methotrexate in urine samples.

    Science.gov (United States)

    Muñoz de la Peña, A; Durán Merás, I; Jiménez Girón, A

    2006-08-01

    First-, second- and third-order calibration methods were investigated for the simultaneous determination of folic acid and methotrexate. The interest in the determination of these compounds is related to the fact that methotrexate inhibits the body's absorption of folic acid and prolonged treatment with methotrexate may lead to folic acid deficiency, and to the use of folic acid to cope with toxic side effects of methotrexate. Both analytes were converted into highly fluorescent compounds by oxidation with potassium permanganate, and the kinetics of the reaction was continuously monitored by recording the kinetics curves of fluorescence emission, the evolution with time of the emission spectra and the excitation-emission matrices (EEMs) of the samples at different reaction times. Direct determination of mixtures of both drugs in urine was accomplished on the basis of the evolution of the kinetics of EEMs by fluorescence measurements and four-way parallel-factor analysis (PARAFAC) or multiway partial least squares (N-PLS) chemometric calibration. The core consistency diagnostic (CORCONDIA) was employed to determine the correct number of factors in PARAFAC and the procedure converged to a choice of three factors, attributed to folic acid, methotrexate and to the sum of fluorescent species present in the urine.

  9. RP-HPLC-UV method coupled with post-column iodine-azide reaction for determination of free captopril in urine samples.

    Science.gov (United States)

    Łuczak, Adam; Zakrzewski, Robert; Dobrogowski, Miłosz

    2012-06-01

    A free urinary captopril is measured indirectly employing the iodine-azide reaction in post-column mode. The pre-clean-up and/or derivatization step is needless, so that the method is adequate for rapid captopril determination in the urine samples and its monitoring at clinical trial. Captopril is separated on a C4 column by the eluate composed of sodium azide solution (4% [w/v], pH 5.8), acetonitrile and water at a ratio of 50:5:45 (v/v/v). The linearity exists in the range from 0.06 to 2.25 µmol/ml of urine. LOD and LOQ receive 0.03 and 0.06 µmol/ml of urine, respectively. Inter-day precision and accuracy of measurements of the captopril-spiked urine samples were 9, 8 and 5%, and 104, 107 and 105%, respectively, for 0.060 (low level), 0.50 (medium level) and 1.25 (high level) µmol/ml of urine. Captopril content was determined in real urine samples delivered from patients treated with this drug.

  10. Detection of recombinant EPO in blood and urine samples with EPO WGA MAIIA, IEF and SAR-PAGE after microdose injections.

    Science.gov (United States)

    Dehnes, Yvette; Shalina, Alexandra; Myrvold, Linda

    2013-01-01

    The misuse of microdoses of performance enhancing drugs like erythropoietin (EPO) constitutes a major challenge in doping analysis. When injected intravenously, the half-life of recombinant human EPO (rhEPO) like epoetin alfa, beta, and zeta is only a few hours and hence, the window for direct detection of rhEPO in urine is small. In order to investigate the detection window for rhEPO directly in blood and urine with a combined affinity chromatography and lateral flow immunoassay (EPO WGA MAIIA), we recruited nine healthy people who each received six intravenously injected microdoses (7.5 IU/kg) of NeoRecormon (epoetin beta) over a period of three weeks. Blood and urine samples were collected in the days following the injections and analyzed with EPO WGA MAIIA as well as the current validated methods for rhEPO; isoelectric focusing (IEF) and sarcosyl polyacrylamide gel electrophoresis (SAR-PAGE). For samples collected 18 h after a microdose, the sensitivity of the EPO WGA MAIIA assay was 100% in plasma and 87.5% in urine samples at the respective 98% specificity threshold levels. In comparison, the sensitivity in plasma and urine was 75% and 100%, respectively, with IEF, and 87.5% in plasma and 100% in urine when analyzed with SAR-PAGE. We conclude that EPO WGA MAIIA is a sensitive assay for the detection of rhEPO, with the potential of being a fast, supplemental screening assay for use in doping analysis.

  11. Surface-activated chemical ionization ion trap mass spectrometry in the analysis of amphetamines in diluted urine samples.

    Science.gov (United States)

    Cristoni, Simone; Bernardi, Luigi Rossi; Gerthoux, Piermario; Gonella, Elisabetta; Mocarelli, Paolo

    2004-01-01

    A new ionization method, named surface-activated chemical ionization (SACI), was employed for the analysis of five amphetamines (3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDE), amphetamine and methamphetamine) by ion trap mass spectrometry. The results so obtained have been compared with those achieved by using atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) using the same instrument, clearly showing that SACI is the most sensitive of the three. The limit of detection and linearity range for SACI were compared with those obtained using APCI and ESI, showing that the new SACI approach provides the best results for both criteria. SACI was used to analyze MDA, MDMA MDE, amphetamine and methamphetamine in four urine samples, and the quantitation results are compared with those achieved using ESI.

  12. Develpoment of a procedure for the determination of chromium in samples of urine and serum by neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Buettner, I. (Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry); Hamm, V. (Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry); Knoechel, A. (Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry); Sen Gupta, R. (Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry)

    1993-06-01

    Since the mid-fifties the possibility of a causal relationship between deficient chromium and insulin metabolism and the manifestation of certain varieties of diabetes mellitus has been presumed. The determination of the chromium status under pathophysiological conditions may be helpful for the study of this problem. For these purposes an analytical procedure as reference system was developed which allows the determination of chromium in biological matrices down to the concentration of 0.33 ng/ml. It is based on NAA and is used in the framework of a commonly used procedure based on GF-AAS. For its application blood and urine samples are freeze-dried and irradiated. After wet digestion with HNO[sub 3] in a microwave combustion system chromium is separated for measurement from the matrix nuclides with the help of the ion-exchanger Cellex-P. THe individual steps of the procedure were evaluated by means of tracer experiments. (orig.)

  13. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, S. E.; Freese, R.; Cornett, Claus

    2000-01-01

    by column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring...... of variation for the analysis of the 12 different flavonoids in quality control urine samples were 12.3% on average (range 11.0-13.7%, n = 24, reproducibility) and the repeatability of the assay were 5.0% (mean, range 0.1-14.8%, it = 12). A subset of 10 urine samples from a human dietary intervention study...

  14. Method for Determination of Neptunium in Large-Sized Urine Samples Using Manganese Dioxide Coprecipitation and 242Pu as Yield Tracer

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel method for bioassay of large volumes of human urine samples using manganese dioxide coprecipitation for preconcentration was developed for rapid determination of 237Np. 242Pu was utilized as a nonisotopic tracer to monitor the chemical yield of 237Np. A sequential injection extraction...... to 100% and high separation capacity of processing up to 5 L of human urine samples. The MnO2 coprecipitation process is simple and straightforward in which a batch (8–12) of samples can be pretreated within 4 h (i.e.,

  15. A multiclass method for the analysis of endocrine disrupting chemicals in human urine samples. Sample treatment by dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Vela-Soria, F; Ballesteros, O; Zafra-Gómez, A; Ballesteros, L; Navalón, A

    2014-11-01

    The population is continuously exposed to endocrine disrupting chemicals (EDCs). This has influenced an increase in diseases and syndromes that are more frequent nowadays. Therefore, it is necessary to develop new analytical procedures to evaluate the exposure with the ultimate objective of establishing, in an accurate way, relationships between EDCs and harmful health effects. In the present work, a new method based on a sample treatment by dispersive liquid-liquid microextraction (DLLME) for the extraction of six parabens (methyl-, ethyl-, isopropyl-, propyl-, isobutyl and butylparaben), six benzophenones (benzophenone-1, benzophenone-2, benzophenone-3, benzophenone-6, benzophenone-8 and 4-hydroxybenzophenone) and two bisphenols (bisphenol A and bisphenol S) in human urine samples, followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis is proposed. An enzymatic treatment allows determining the total content of the target EDCs. The extraction parameters were accurately optimized using multivariate optimization strategies. Ethylparaben ring-(13)C6 and bisphenol A-d16 were used as surrogates. Found limits of quantification ranging from 0.2 to 0.5 ng mL(-1) and inter-day variability (evaluated as relative standard deviation) ranging from 2.0% to 14.9%. The method was validated using matrix-matched standard calibration followed by a recovery assay with spiked samples. Recovery rates ranged from 94% to 105%. A good linearity, for concentrations up to 300 ng mL(-1) for parabens and 40 ng mL(-1) for benzophenones and bisphenols, respectively, was obtained. The method was satisfactorily applied for the determination of target compounds in human urine samples from 20 randomly selected individuals.

  16. Storage stability studies for tributyltin determination in human urine samples using headspace solid-phase microextraction and gas chromatography mass spectrometry.

    Science.gov (United States)

    Zachariadis, G A; Tzollas, N M; Nikolaou, M; Rosenberg, E

    2013-03-01

    A headspace solid-phase micro-extraction (HS-SPME) method was employed in order to study the effect of storage conditions of human urine samples spiked with tributyltin (TBT) using gas chromatography and mass spectrometry. To render the analyte more volatile, the derivatization (ethylation) was made in situ by sodium tetraethylborate (NaBEt(4) ), which was added directly to dilute unpreserved urine samples and in buffers of similar acidity. The stability of TBT in human urine matrix was compared with the stability of TBT in buffer solutions of similar pH value. Critical parameters of storage conditions such as temperature and time, which affect the stability of TBT in this kind of matrix, were examined extensively. The tests showed that the stability of TBT remains practically satisfactory for a maximum of 2 days of storage either at +4 or 20°C. Greater variations were observed in the concentration of TBT in human urine samples at +4°C and lower ones at -20°C over a month's storage. The freeze-thaw cycles have negative effect on the stability and should be kept to a minimum. The results from spiked urine samples are also discussed in comparison to those acquired from buffer solutions of equal TBT concentration.

  17. Determination of terbuthylazine and desethylterbuthylazine in human urine and hair samples by eletrospray ionization-liquid chromatography/triple quadrupole mass spectrometry.

    Science.gov (United States)

    Mercadante, Rosa; Polledri, Elisa; Fustinoni, Silvia

    2012-08-01

    Terbuthylazine (TBA) is a widely applied herbicide and an environmental contaminant. Following its use, humans, such as agricultural workers and rural residents, may be exposed. An isotope-dilution liquid chromatography coupled to electrospray-tandem mass spectrometry method for the determination of TBA, and its metabolite desethylterbuthylazine (DET) in human urine and hair was developed and validated. Under the optimised conditions, analytes were extracted from urine using a solid phase cartridge or from hair by sonication in methanol. Analytes were separated using a C18 reversed-phase chromatographic column and quantified, after positive ionization using a heated electrospray source, by a triple quadrupole mass detector in the selected reaction monitoring mode. Validation showed linear dynamic ranges up to 100 μg/L or 5.00 ng/mg hair, inter- and intra-run precisions <7%, and accuracies within 12% of spiked concentrations. Limits of quantification were 0.25 μg/L in urine and 0.01 ng/mg hair for both TBA and DET. Matrix effect evaluation showed that the isotope dilution approach allowed for the control of bias sources. TBA and DET were determined in specimens of agriculture workers exposed to TBA using the validated method. Hair samples contained TBA levels in the low nanogram per milligram range, and urine samples contained DET levels in the low microgram per liter range. Conversely, TBA levels in urine samples and DET levels in hair samples were always below the limit of quantification.

  18. CTEPP STANDARD OPERATING PROCEDURE FOR EXTRACTING AND PREPARING URINE SAMPLES FOR ANALYSIS OF HYDROXY POLYCYCLIC AROMATIC HYDROCARBONS, PENTACHLOROPHENOL AND 2,4-D (SOP-5.21)

    Science.gov (United States)

    The method for extracting and preparing urine samples for analysis of hydroxy-polycyclic aromatic hydrocarbons, pentachlorophenol and 2,4-D is summarized in this SOP. It covers the extraction, concentration and methylation of samples that are to be analyzed by gas chromatography/...

  19. Use of fission track analysis technique for the determination of MicroBequerel level of 239Pu in urine samples from radiation workers handling MOX fuel.

    Science.gov (United States)

    Yadav, J R; Rao, D D; Kumar, Ranjeet; Aggarwal, S K

    2011-07-01

    Fission track analysis (FTA) technique for the determination of (239)Pu excreted through urine has been standardized using blank samples, tracer and (239)Pu spikes. Double stage anion exchange separation protocol has been applied and an average radiochemical recovery of (239)Pu of 18% was obtained. An average track registration efficiency of 11 tracks per μBq of (239)Pu, irradiated to 0.35×10(17) neutron fluence was established. Reagent blank urine samples from 11 controlled subjects were analyzed by FTA and an average of 149±14 tracks was obtained. Minimum detectable activity of 34μBqL(-1) of urine sample was obtained and will be useful for monitoring chronic exposure cases handling MOX fuel.

  20. Evaluation of banked urine samples for the detection of circulating anodic and cathodic antigens in Schistosoma mekongi and S. japonicum infections: a proof-of-concept study.

    Science.gov (United States)

    van Dam, Govert J; Odermatt, Peter; Acosta, Luz; Bergquist, Robert; de Dood, Claudia J; Kornelis, Dieuwke; Muth, Sinuon; Utzinger, Jürg; Corstjens, Paul L A M

    2015-01-01

    In Asia, Schistosoma japonicum is the predominant schistosome species, while Schistosoma mekongi is confined to limited foci in Cambodia and Lao People's Democratic Republic. While the People's Republic of China has been successful in controlling schistosomiasis, the disease remains a major public health issue in other areas. In order to prioritise intervention areas, not only accurate diagnosis is important but also other factors, such as practicality, time-efficiency and cost-effectiveness, since they strongly influence the success of control programmes. To evaluate the highly specific urine-based assays for the schistosome circulating cathodic antigen (CCA) and the circulating anodic antigen (CAA), banked urine samples from Cambodia (n=106) and the Philippines (n=43) were examined by the upconverted phosphor lateral flow (UCP-LF) CAA assay and the point-of-care (POC)-CCA urine assay. Based on 250 μl urine samples, UCP-LF CAA sensitivity outcomes surpassed a single stool examination by the Kato-Katz technique. The banked urine samples in the current study did not allow the evaluation of larger volumes, which conceivably should deliver considerably higher readings. The sensitivity of a single urine POC-CCA was in the same order as that of a single Kato-Katz thick smear examination, while the sensitivity approached that of triplicate Kato-Katz when a combination of both CAA and CCA assays was used. The promising results from the current proof-of-concept study call for larger investigations that will determine the accuracy of the urine-based CCA and CAA assays for S. mekongi and S. japonicum diagnosis.

  1. Rapid determination of nine parabens and seven other environmental phenols in urine samples of German children and adults.

    Science.gov (United States)

    Moos, Rebecca K; Angerer, Jürgen; Wittsiepe, Jürgen; Wilhelm, Michael; Brüning, Thomas; Koch, Holger M

    2014-11-01

    We developed a fast, selective and sensitive on-line LC/LC-MS/MS method for the simultaneous determination of nine parabens and seven environmental phenols in urine. Parabens are widely used as antimicrobial preservatives. Bisphenol A, triclosan, triclocarban, 2-phenylphenol, and benzophenones are used inter alia in disinfectants, sunscreens and in polymers. Some of these substances are suspected endocrine disruptors. Limits of quantification and analytical quality criteria fully met the needs for determining exposure levels occurring in the general population. We analyzed 157 spot urine samples from the general German population (59 females, 39 males and 59 children). For the parabens, we found methyl, ethyl and n-propyl paraben with high detection rates (77-98%), followed by n-butyl (36%), iso-butyl (17%), iso-propyl (3%) and benzyl paraben (3%). We detected no pentyl and heptyl paraben. Urinary concentrations were highest for methyl paraben (median 24.5 μg/L; 95th percentile 379 μg/L) followed by ethyl (1.4 μg/L; 35.2 μg/L) and n-propyl paraben (1.2 μg/L; 68.1 μg/L). Other environmental phenols with high detection rates were BPA (95%), triclosan (45%) and benzophenone 1 and 3 (26%). For most of the parabens/environmental phenols we found higher urinary levels in females than in males or children, probably due to differences in (personal care) product use. However, high levels (in the mg/L range) were also observed in children. Exposure to the above substances is occurring worldwide. Differences between countries do seem to exist and might be caused by different product compositions or different use habits. Human metabolism data is urgently needed to extrapolate from urinary biomarker levels to doses actually taken up. Copyright © 2014 Elsevier GmbH. All rights reserved.

  2. Rapid extraction and determination of amphetamines in human urine samples using dispersive liquid-liquid microextraction and solidification of floating organic drop followed by high performance liquid chromatography.

    Science.gov (United States)

    Ahmadi-Jouibari, Toraj; Fattahi, Nazir; Shamsipur, Mojtaba

    2014-06-01

    A novel, rapid, simple and sensitive dispersive liquid-liquid microextraction method based on the solidification of floating organic drop (DLLME-SFO) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was used to determine amphetamine and methamphetamine in urine samples. The factors affecting the extraction efficiency of DLLME-SFO such as the kind and volume of the extraction and the disperser solvents, effect of concentration of K2CO3 and extraction time were investigated and the optimal extraction conditions were established. Under the optimum conditions (extraction solvent: 30.0μl 1-undecanol; disperser solvent: 300μl acetonitrile; buffer concentration: 2% (w/v) K2CO3 and extraction time: 1min), calibration curves are linear in the range of 10-3000μgl(-1) and limit of detections (LODs) are in the range of 2-8μgl(-1). The relative standard deviations (RSDs) for 100μgl(-1) of amphetamine and methamphetamine in diluted urine are in the range of 6.2-7.8% (n=7). The method was successfully applied for the determination of amphetamine and methamphetamine in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 87.8-113.2%. The obtained results show that DLLME-SFO combined with HPLC-UV is a fast and simple method for the determination of amphetamine and methamphetamine in urine.

  3. Rapid confirmation of enzyme multiplied immunoassay technique (EMIT) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD).

    Science.gov (United States)

    Verebey, K; DePace, A

    1989-01-01

    A rapid gas-liquid chromatographic (GLC) method was developed for the confirmation of benzoylecgonine (BE) positive urine samples screened by the enzyme multiplied immunoassay technique (EMIT) assay. The procedure is performed by solvent extraction of BE from 0.1 or 0.2 mL of urine, followed by an aqueous wash of the solvent and evaporation. The dried residue was derivatized with 50 microL of pentafluoropropionic anhydride and 25 microL of pentafluoropropropanol at 90 degrees C for 15 min. The derivatizing reagents were evaporated to dryness, and the derivatized BE, and cocaine if present, were reconstituted and injected into the gas chromatograph. The column was a 15-m by 0.2-mm fused silica capillary column, coated with 0.25 micron of DB-1, terminating in a nitrogen phosphorus detector (NPD). Cocaine and the pentafluoro BE derivatives retention times were 3.2 and 2.6 min, respectively. Nalorphine was used as reference or internal standard with a retention time of 4.78 min. The complete procedure can be performed in approximately 1.5 h. The EMIT cutoff between positive and negative urine samples is 300 ng/mL of BE. The lower limit of sensitivity of this method is 25 ng of BE extracted from urine. Validation studies resulted in confirmation of 101 out of 121 EMIT cocaine positive urine samples that could not be confirmed by thin-layer chromatography (TLC). This represents 84% confirmation efficiency.

  4. An analysis of workers' tritium concentration in urine samples as a function of time after intake at Korean pressurised heavy water reactors.

    Science.gov (United States)

    Kim, Hee Geun; Kong, Tae Young

    2012-12-01

    In general, internal exposure from tritium at pressurised heavy water reactors (PHWRs) accounts for ∼20-40 % of the total radiation dose. Tritium usually reaches the equilibrium concentration after a few hours inside the body and is then excreted from the body with an effective half-life in the order of 10 d. In this study, tritium metabolism was reviewed using its excretion rate in urine samples of workers at Korean PHWRs. The tritium concentration in workers' urine samples was also measured as a function of time after intake. On the basis of the monitoring results, changes in the tritium concentration inside the body were then analysed.

  5. Strong-LAMP: A LAMP Assay for Strongyloides spp. Detection in Stool and Urine Samples. Towards the Diagnosis of Human Strongyloidiasis Starting from a Rodent Model

    Science.gov (United States)

    Gandasegui, Javier; Bajo Santos, Cristina; López-Abán, Julio; Saugar, José María; Rodríguez, Esperanza; Vicente, Belén; Muro, Antonio

    2016-01-01

    Background Strongyloides stercoralis, the chief causative agent of human strongyloidiasis, is a nematode globally distributed but mainly endemic in tropical and subtropical regions. Chronic infection is often clinically asymptomatic but it can result in severe hyperinfection syndrome or disseminated strongyloidiasis in immunocompromised patients. There is a great diversity of techniques used in diagnosing the disease, but definitive diagnosis is accomplished by parasitological examination of stool samples for morphological identification of parasite. Until now, no molecular method has been tested in urine samples as an alternative to stool samples for diagnosing strongyloidiasis. This study aimed to evaluate the use of a new molecular LAMP assay in a well-established Wistar rat experimental infection model using both stool and, for the first time, urine samples. The LAMP assay was also clinically evaluated in patients´ stool samples. Methodology/Principal Findings Stool and urine samples were obtained daily during a 28-day period from rats infected subcutaneously with different infective third-stage larvae doses of S. venezuelensis. The dynamics of parasite infection was determined by daily counting the number of eggs per gram of feces from day 1 to 28 post-infection. A set of primers for LAMP assay based on a DNA partial sequence in the 18S rRNA gene from S. venezuelensis was designed. The set up LAMP assay (namely, Strong-LAMP) allowed the sensitive detection of S. venezuelensis DNA in both stool and urine samples obtained from each infection group of rats and was also effective in S. stercoralis DNA amplification in patients´ stool samples with previously confirmed strongyloidiasis by parasitological and real-time PCR tests. Conclusions/Significance Our Strong-LAMP assay is an useful molecular tool in research of a strongyloidiasis experimental infection model in both stool and urine samples. After further validation, the Strong-LAMP could also be potentially

  6. Nappy pad urine samples for investigation and treatment of UTI in young children: the ‘DUTY’ prospective diagnostic cohort study

    Science.gov (United States)

    Butler, Christopher C; Sterne, Jonathan AC; Lawton, Michael; O’Brien, Kathryn; Wootton, Mandy; Hood, Kerenza; Hollingworth, William; Little, Paul; Delaney, Brendan C; van der Voort, Judith; Dudley, Jan; Birnie, Kate; Pickles, Timothy; Waldron, Cherry-Ann; Downing, Harriet; Thomas-Jones, Emma; Lisles, Catherine; Rumsby, Kate; Durbaba, Stevo; Whiting, Penny; Harman, Kim; Howe, Robin; MacGowan, Alasdair; Fletcher, Margaret; Hay, Alastair D

    2016-01-01

    Background The added diagnostic utility of nappy pad urine samples and the proportion that are contaminated is unknown. Aim To develop a clinical prediction rule for the diagnosis of urinary tract infection (UTI) based on sampling using the nappy pad method. Design and setting Acutely unwell children <5 years presenting to 233 UK primary care sites. Method Logistic regression to identify independent associations of symptoms, signs, and urine dipstick test results with UTI; diagnostic utility quantified as area under the receiver operator curves (AUROC). Nappy pad rule characteristics, AUROC, and contamination, compared with findings from clean-catch samples. Results Nappy pad samples were obtained from 3205 children (82% aged <2 years; 48% female), culture results were available for 2277 (71.0%) and 30 (1.3%) had a UTI on culture. Female sex, smelly urine, darker urine, and the absence of nappy rash were independently associated with a UTI, with an internally-validated, coefficient model AUROC of 0.81 (0.87 for clean-catch), which increased to 0.87 (0.90 for clean-catch) with the addition of dipstick results. GPs’ ‘working diagnosis’ had an AUROC 0.63 (95% confidence intervals [CI] = 0.53 to 0.72). A total of 12.2% of nappy pad and 1.8% of clean-catch samples were ‘frankly contaminated’ (risk ratio 6.66; 95% CI = 4.95 to 8.96; P<0.001). Conclusion Nappy pad urine culture results, with features that can be reported by parents and dipstick tests, can be clinically useful, but are less accurate and more often contaminated compared with clean-catch urine culture. PMID:27364678

  7. Fast and reliable method for As speciation in urine samples containing low levels of As by LC-ICP-MS: Focus on epidemiological studies.

    Science.gov (United States)

    Carioni, V M O; McElroy, J A; Guthrie, J M; Ngwenyama, R A; Brockman, J D

    2017-04-01

    The speciation analysis of As in urine samples can provide important information for epidemiological studies. Considering that these studies involve hundreds or thousands of samples, a fast and reliable method using a simple LC system with short-length mixed bed ion exchange chromatographic column coupled to ICP-MS for As speciation in human urine samples was developed in this work. Separation of AB+TMAO, DMA, AC, MMA and As(III)+As(V) was accomplished within 5min with good resolution when ammonium carbonate solutions were used as mobile phases and H2O2 was added to samples to quantitatively convert As(III)-As(V). Repeatability studies yielded RSD values from 2.0% to 4.8% for all species evaluated. Limits of detection (LOD) for As species ranged from 0.003 to 0.051ngg(-1). Application of the method to human urine samples from a non-contaminated area showed that the sum of species measured corresponded to 62-125% of the total As in the sample. The recovery values for these species in urine SRM 2669 were in the range of 89-112% and demonstrated the suitability of the proposed method for epidemiological studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Detection and genotyping of human papillomavirus in urine samples from unvaccinated male and female adolescents in Italy.

    Science.gov (United States)

    Bianchi, Silvia; Frati, Elena Rosanna; Panatto, Donatella; Martinelli, Marianna; Amicizia, Daniela; Zotti, Carla Maria; Martinese, Morena; Bonanni, Paolo; Boccalini, Sara; Coppola, Rosa Cristina; Masia, Giuseppina; Meloni, Angelo; Castiglia, Paolo; Piana, Andrea; Gasparini, Roberto; Tanzi, Elisabetta

    2013-01-01

    The introduction of vaccination against Human Papillomavirus (HPV) in adolescent girls in 2006 has focused virological surveillance on this age group. As few studies have evaluated HPV infections in young populations, further data are needed in order to improve and extend prophylactic policy and to monitor epidemiological changes. The present study aimed at evaluating overall and type-specific HPV prevalence in both female and male adolescents in Italy. HPV DNA detection and genotyping was performed on urine samples collected from 870 unvaccinated adolescents (369 females, 501 males, 11-18 years of age) in five cities in Italy. Following DNA extraction by means of a commercial kit (NucliSENS(®)-miniMAG(®), bioMérieux), the L1 gene fragment was PCR amplified and genotyped by restriction fragment length polymorphism analysis. HPV DNA was detected in 1.5% of all samples, and in 3% and 0.4% of samples from females and males, respectively. In approximately 70% of HPV DNA positive adolescents, the infection was due to a single genotype, with 88.9% of genotypes belonging to the HR-clade. The only two HPV-positive boys (14 and 18 years old) had HPV-70 genotype. Only one of the 11 HPV-infected girls was in the 11-14 age-group. HPV prevalence was 4.2% in girls aged 15-18 years and 60% of infections were due to vaccine types HPV-16 or HPV-6/-11. This is one of the few studies, the first conducted in Italy, on HPV infection in adolescents. Urine testing is the easier way of detecting HPV infection in younger populations. Our data revealed a very low HPV prevalence, and no infections were observed in the 12-year-old vaccine target population. The majority of infections were seen in females aged 15-18 years. Overall, more than 50% and 30% of the potentially persistent HPV infections detected in this group could have been prevented by the quadrivalent and the bivalent vaccines, respectively.

  9. Detection and genotyping of human papillomavirus in urine samples from unvaccinated male and female adolescents in Italy.

    Directory of Open Access Journals (Sweden)

    Silvia Bianchi

    Full Text Available The introduction of vaccination against Human Papillomavirus (HPV in adolescent girls in 2006 has focused virological surveillance on this age group. As few studies have evaluated HPV infections in young populations, further data are needed in order to improve and extend prophylactic policy and to monitor epidemiological changes. The present study aimed at evaluating overall and type-specific HPV prevalence in both female and male adolescents in Italy. HPV DNA detection and genotyping was performed on urine samples collected from 870 unvaccinated adolescents (369 females, 501 males, 11-18 years of age in five cities in Italy. Following DNA extraction by means of a commercial kit (NucliSENS(®-miniMAG(®, bioMérieux, the L1 gene fragment was PCR amplified and genotyped by restriction fragment length polymorphism analysis. HPV DNA was detected in 1.5% of all samples, and in 3% and 0.4% of samples from females and males, respectively. In approximately 70% of HPV DNA positive adolescents, the infection was due to a single genotype, with 88.9% of genotypes belonging to the HR-clade. The only two HPV-positive boys (14 and 18 years old had HPV-70 genotype. Only one of the 11 HPV-infected girls was in the 11-14 age-group. HPV prevalence was 4.2% in girls aged 15-18 years and 60% of infections were due to vaccine types HPV-16 or HPV-6/-11. This is one of the few studies, the first conducted in Italy, on HPV infection in adolescents. Urine testing is the easier way of detecting HPV infection in younger populations. Our data revealed a very low HPV prevalence, and no infections were observed in the 12-year-old vaccine target population. The majority of infections were seen in females aged 15-18 years. Overall, more than 50% and 30% of the potentially persistent HPV infections detected in this group could have been prevented by the quadrivalent and the bivalent vaccines, respectively.

  10. Urine culture

    Science.gov (United States)

    Culture and sensitivity - urine ... when urinating. You also may have a urine culture after you have been treated for an infection. ... when bacteria or yeast are found in the culture. This likely means that you have a urinary ...

  11. An efficient sample preparation method for high-throughput analysis of 15(S)-8-iso-PGF2α in plasma and urine by enzyme immunoassay.

    Science.gov (United States)

    Bielecki, A; Saravanabhavan, G; Blais, E; Vincent, R; Kumarathasan, P

    2012-01-01

    Although several methods have been reported on the analysis of the oxidative stress marker 15(S)-8-iso-prostaglandin-F2alpha (8-iso-PGF2α) in biological fluids, they either involve extensive sample preparation and costly technology or require high sample volume. This study presents a sample preparation method that utilizes low sample volume for 8-iso-PGF2α analysis in plasma and urine by an enzyme immunoassay (EIA). In brief, 8-iso-PGF2α in deproteinized plasma or native urine sample is complexed with an antibody and then captured by molecular weight cut-off filtration. This method was compared with two other sample preparation methods that are typically used in the analysis of 8-iso-PGF2α by EIA: Cayman's affinity column purification method and solid-phase extraction on C-18. The immunoaffinity purification method described here was superior to the other two sample preparation methods and yielded recovery values of 99.8 and 54.1% for 8-iso-PGF2α in plasma and urine, respectively. Analytical precision (relative standard deviation) was ±5% for plasma and ±15% for urine. The analysis of healthy human plasma and urine resulted in basal 8-iso-PGF2α levels of 31.8 ± 5.5 pg/mL and 2.9 ± 2.0 ng/mg creatinine, respectively. The robustness and analytical performance of this method makes it a promising tool for high-throughput screening of biological samples for 8-iso-PGF2α.

  12. Iridium oxide pH sensor for biomedical applications. Case urea-urease in real urine samples.

    Science.gov (United States)

    Prats-Alfonso, Elisabet; Abad, Llibertat; Casañ-Pastor, Nieves; Gonzalo-Ruiz, Javier; Baldrich, Eva

    2013-01-15

    This work demonstrates the implementation of iridium oxide films (IROF) grown on silicon-based thin-film platinum microelectrodes, their utilization as a pH sensor, and their successful formatting into a urea pH sensor. In this context, Pt electrodes were fabricated on Silicon by using standard photolithography and lift-off procedures and IROF thin films were growth by a dynamic oxidation electrodeposition method (AEIROF). The AEIROF pH sensor reported showed a super-Nerstian (72.9±0.9mV/pH) response between pH 3 and 11, with residual standard deviation of both repeatability and reproducibility below 5%, and resolution of 0.03 pH units. For their application as urea pH sensors, AEIROF electrodes were reversibly modified with urease-coated magnetic microparticles (MP) using a magnet. The urea pH sensor provided fast detection of urea between 78μM and 20mM in saline solution, in sample volumes of just 50μL. The applicability to urea determination in real urine samples is discussed.

  13. Surface molecularly imprinted silica for selective solid-phase extraction of biochanin A, daidzein and genistein from urine samples.

    Science.gov (United States)

    Chrzanowska, Anna M; Poliwoda, Anna; Wieczorek, Piotr P

    2015-05-01

    Selective molecularly imprinted silica polymer (SiO2MIP) for extraction of biochanin A, daidzein and genistein was synthesized using the surface molecular imprinting technique with the silica gel as a support. Biochanin A (BCA) was used as a template, 3-aminopropyltriethoxysilane (APTES) as a functional monomer, and tetraethoxysilicane (TEOS) as a cross-linker. Non-imprinted polymer with the sol-gel process (SiO2NIP) was also prepared for comparison. The synthesized polymers were characterized by Fourier transform infrared spectrometry (FTIR), scanning electron microscopy (SEM) and a standard Brunauer-Emett-Teller (BET) and Barret-Joyner-Halenda (BJH) analysis. The obtained results indicated the structural differences between imprinted and non-imprinted polymers. Finally, the SiO2MIP and SiO2NIP were adopted as the adsorbents of solid phase extraction for isolation and preconcentration of biochanin A and its structural analogues-daidzein and genistein from aqueous and urine samples. The performance analysis revealed that SiO2MIP displayed better affinity to the three investigated isoflavones compared with SiO2NIP. The recoveries of spiked samples for studied analytes ranged from 65.7% to 102.6% for molecularly imprinted silica polymer and 8.9-16.0% for non-imprinted sorbents.

  14. Urinary vanillylmandelic acid and homovanillic acid levels in randomly-sampled urine for the mass screening of neuroblastoma.

    Science.gov (United States)

    Nishi, M; Miyake, H; Takeda, T; Takasugi, N; Hanai, J; Kawai, T

    1990-09-01

    Employing 421 urine samples taken randomly from normal infants and 294 samples from infants with neuroblastoma, we investigated the application of values of vanillylmandelic acid (VMA), homovanillic acid (HVA) and square root of VMA2 + HVA2 to discriminate between patients and normal infants. The establishment of an HVA cut-off level is virtually impossible because of its low sensitivity. In contrast, VMA sensitivity is high, and that of square root of VMA2 + HVA2 is very similar to that of VMA although it includes HVA. Although VMA appears to be able to discriminate well, discrimination employing VMA alone would be dangerous because cases with normal VMA and abnormal HVA would be missed, especially in the first screening for which a mechanical discrimination is performed. Overlooking such cases can be avoided by the adoption of the function square root of VMA2 + HVA2. The present study suggests that the combined use of variables can be more effective than using them separately.

  15. Determination of Parent and Hydroxy PAHs in Personal PM2.5 and Urine Samples Collected During Native American Fish Smoking Activities

    Science.gov (United States)

    Motorykin, Oleksii; Schrlau, Jill; Jia, Yuling; Harper, Barbara; Harris, Stuart; Harding, Anna; Stone, David; Kile, Molly; Sudakin, Daniel; Massey Simonich, Staci L.

    2014-01-01

    A method was developed for the measurement of 19 parent PAHs (PAHs) and 34 hydroxylated PAHs (OH-PAHs) in urine and personal air samples of particulate matter less than 2.5 um in diameter (PM2.5) using GC-MS and validated using NIST SRM 3672 (Organic Contaminants in Smoker’s Urine) and SRM 3673 (Organic Contaminants in Nonsmoker’s Urine). The method was used to measure PAHs and OH-PAHs in urine and personal PM2.5 samples collected from the operators of two different fish smoking facilities (tipi and smoke shed) burning two different wood types (alder and apple) on the Confederated Tribes of Umatilla Indian Reservation (CTUIR) while they smoked salmon. Urine samples were spiked with β-glucuronidase/arylsulfatase to hydrolyze the conjugates of OH-PAHs and the PAHs and OH-PAHs were extracted using Plexa and C18 solid phases, in series. The 34OH-PAHs were derivatized using MTBSTFA, and the mixture was measured by GC-MS. The personal PM2.5samples were extracted using pressurized liquid extraction, derivatized with MTBSTFA and analyzed by GC-MS for PAHs and OH-PAHs. Fourteen isotopically labeled surrogates were added to accurately quantify PAHs and OH-PAHs in the urine and PM2.5 samples and three isotopically labeled internal standards were used to calculate the recovery of the surrogates. Estimated detection limits in urine ranged from 6.0 to 181 pg/ml for OH-PAHs and from 3.0 to 90 pg/ml for PAHs, and, in PM2.5, they ranged from 5.2 to 155 pg/m3 for OH-PAHs and from 2.5 to 77 pg/m3 for PAHs. The results showed an increase in OH-PAH concentrations in urine after 6 hours offish smoking and an increase in PAH concentrations in air within each smoking facility. In general, the PAH exposure in the smoke shed was higher than in the tipi and the PAH exposure from burning apple wood was higher than burning alder. PMID:25461072

  16. Monoclonal antibody-based dipstick assay: a reliable field applicable technique for diagnosis of Schistosoma mansoni infection using human serum and urine samples.

    Science.gov (United States)

    Demerdash, Zeinab; Mohamed, Salwa; Hendawy, Mohamed; Rabia, Ibrahim; Attia, Mohy; Shaker, Zeinab; Diab, Tarek M

    2013-02-01

    A field applicable diagnostic technique, the dipstick assay, was evaluated for its sensitivity and specificity in diagnosing human Schistosoma mansoni infection. A monoclonal antibody (mAb) against S. mansoni adult worm tegumental antigen (AWTA) was employed in dipstick and sandwich ELISA for detection of circulating schistosome antigen (CSA) in both serum and urine samples. Based on clinical and parasitological examinations, 60 S. mansoni-infected patients, 30 patients infected with parasites other than schistosomiasis, and 30 uninfected healthy individuals were selected. The sensitivity and specificity of dipstick assay in urine samples were 86.7% and 90.0%, respectively, compared to 90.0% sensitivity and 91.7% specificity of sandwich ELISA. In serum samples, the sensitivity and specificity were 88.3% and 91.7% for dipstick assay vs. 91.7% and 95.0% for sandwich ELISA, respectively. The diagnostic efficacy of dipstick assay in urine and serum samples was 88.3% and 90.0%, while it was 90.8% and 93.3% for sandwich ELISA, respectively. The diagnostic indices of dipstick assay and ELISA either in serum or in urine were statistically comparable (P>0.05). In conclusion, the dipstick assay offers an alternative simple, rapid, non-invasive technique in detecting CSA or complement to stool examinations especially in field studies.

  17. Survey of False-positive Reactivity of Latex Agglutination Test for Kala-azar (Katex) without Urine Sample Boiling Process in Autoimmune Patients.

    Science.gov (United States)

    Ghatee, Mohammad Amin; Kanannejad, Zahra; Sharifi, Iraj; Askari, Asma; Bamorovat, Mehdi

    2017-06-01

    Latex agglutination test for Kala-azar (KAtex) is an easy, inexpensive, and field-applicable antigen detection test. However, the main drawback of this method is the boiling step applied to remove false positivity of the test. This study was conducted to survey false positivity results of latex agglutination test for KAtex without boiling process in urine of some autoimmune patients. Ninety-two urine samples from autoimmune patients including systemic lupus erythematosus (SLE), rheumatoid arthritis (RA), scleroderma, autoimmune vasculitis, vitiligo, pemphigus and Wagner cases and 20 urine samples from healthy individuals were collected from Kerman Province in Southeastern Iran in 2010-2011. All urine samples were checked by KAtex after boiling for 5 min false positivity rate of the test was surveyed in different healthy and patients groups while boiling process was removed. Rheumatoid factor (RF) then was checked in sera of all cases to evaluate the relationship between RF and KAtex false positivity. All samples represented negative results with KAtex when boiling was performed (100% specificity). Then, 20% positivity was evident in healthy cases. False-positive reactivity was more prominent observed in patient groups than healthy individuals, except in vitiligo. However, a significant difference was only observed in RA group (Pboiling process removal.

  18. High throughput analysis of drugs of abuse in hair by combining purposely designed sample extraction compatible with immunometric methods used for drug testing in urine.

    Science.gov (United States)

    de la Torre, R; Civit, E; Svaizer, F; Lotti, A; Gottardi, M; Miozzo, M

    2010-03-20

    Drug testing in hair usually requires a rather complex sample treatment before drugs are amenable to analysis by either immunological and/or chromatographic coupled to mass spectrometry methods. Immunological methods applied are usually dedicated to hair analysis as analytes present in this matrix are not always the same present in urine. Comedical s.a.s. laboratories recently commercialized reagents (VMA-T) purposely designed for hair sample treatment which are compatible with current immunometric methods used for urine drug testing. This is possible as some analytes (6-MAM and cocaine) present in hair after sample treatment are converted to those detected in urine (morphine and benzoylecgonine). A correlation study for several drug classes performed in two laboratories with 32 clinical and 12 spiked drug free (controls) hair samples shows that implementation of the method on clinical chemistry analyzers is easy and that results obtained by different operators and instruments are comparable and reproducible. The main advantage of VMA-T method is the possibility to simultaneously extract from hair main drug classes, in a period of time lower than 2h and its compatibility with immunological methods applied in urine drug testing.

  19. Extraction and Determination of Zolpidem in Tablets and Urine Samples by Dispersive Liquid-Liquid Microextraction and UV-Vis Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Majid Soleimani

    2016-12-01

    Full Text Available A simple and inexpensive method for Zolpidem determination in tablets and urine samples using dispersive liquidliquid microextraction and ultraviolet-visible spectrophotometry was developed. Experimental parameters affecting the DLLME method such as pH, type and volume of extraction and dispersive solvent were investigated and optimized. Under the optimized conditions, the absorbance was in proportion to Zolpidem concentration in the range of 0.1 - 30 mg/L with a correlation coefficient (R of 0.9972. The limit of detection (LOD was 0.08 mg/L. The relative standard deviation (RSD for real samples were 2.61 %- 3.81 % (n=3. Good recoveries of Zolpidem were obtained in the range of 90–95.25% in tablet samples 76–82.6% in urine samples. Finally, the results shown that the proposed method was successfully applied for the preconcentration and determination of the Zolpidem in real samples.

  20. A novel coated silver ketamine(I electrode for potentiometric determination of ketamine hydrochloride in ampoules and urine samples

    Directory of Open Access Journals (Sweden)

    Hazem M. Abu Shawish

    2014-11-01

    Full Text Available A new ketamine coated silver electrode (KCSE based on ketamine hydrochloride with sodium tetraphenylborate (KT-TPB as electroactive material has been described. The influence of membrane composition, type of solvent mediators, kind of electroactive materials and interfering ions on the sensor was investigated. The sensor displays Nernstian response of 55.8 ± 0.3 mV/decade over the concentration range of 2.5 × 10−6 to 1.0 × 10−2 M with limit of detection of 8.5 × 10−7 M. The coated wire electrode has short response time ∼8 s and it can be used in pH range of 2.6–6.4. The selective coefficients were determined in relation to several inorganic, organic ions, sugars and some common drug excipients. The KCSE electrode was successfully used for the determination of the ketamine content in ampoule and urine samples with satisfactory results. Statistical student’s t-test and F test showed insignificant systematic error between proposed and official methods.

  1. Spectrophotometric Determination of the Trace Amount of Thallium in Water and Urine Samples by Novel Oxidative Coupling Reaction

    Directory of Open Access Journals (Sweden)

    P. Nagaraja

    2009-01-01

    Full Text Available A novel, simple, rapid, sensitive and selective method has been proposed for the trace determination of thallium by spectrophotometric detection. This method is based on the oxidation of MBTH (3-methyl-2-benzothiazolinone hydrazone hydrochloride by thallium(III to form diazonium cation, which couples with IPH (Imipramine hydrochloride in phosphoric acid medium at room temperature giving a blue colored species having a maximum absorption at 635 nm. The reagents and manifold variables influences on the sensitivity were investigated and the optimum reaction conditions have been established. The calibration curve was found to be linear over the range 0.1-5 μg mL-1 with the molar absorptivity and Sandell’s sensitivity of 2.9x104 L mol-1 cm-1, 0.0071 μg cm-2 respectively. The tolerance limit of the method towards various ions usually associated with thallium has been detected. The relative standard deviation for five replicate determination of 2μg mL-1 thallium was 0.47%. The method has been successfully applied for the determination of thallium(ІΙΙ and thallium(I in synthetic, standard reference materials, water and urine samples with satisfactory results. The performance of the proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.

  2. DDT, DDE, and 1-hydroxypyrene levels in children (in blood and urine samples) from Chiapas and Oaxaca, Mexico.

    Science.gov (United States)

    Pérez-Maldonado, Iván N; Trejo-Acevedo, Antonio; Pruneda-Alvarez, Lucia Guadalupe; Gaspar-Ramirez, Octavio; Ruvalcaba-Aranda, Selene; Perez-Vazquez, Francisco Javier

    2013-11-01

    The aim of this study was to evaluate the DDT, DDE, and 1-hydroxypyrene exposure levels of children living in communities located in southeastern Mexico. The study communities were Lacanja and Victoria in Chiapas state and Ventanilla in Oaxaca state. Children living in Lacanja had total blood DDT levels (mean ± SD, 29,039.6 ± 11,261.4 ng/g lipid) that were significantly higher than those of children in Victoria (10,220.5 ± 7,893.1 ng/g lipid) and Ventanilla (11,659.7 ± 6,683.7 ng/g lipid). With respect to the 1-hydroxypyrene levels in urine samples, the levels in Lacanja (4.8 ± 4.1 μg/L or 4.5 ± 3.9 μmol/mol creatinine) and Victoria (4.6 ± 3.8 μg/L or 3.9 ± 3.0 μmol/mol Cr) were significantly higher than levels found in Ventanilla (3.6 ± 1.4 μg/L or 2.5 ± 0.5 μmol/mol Cr). In conclusion, our data indicate high levels of exposure in children living in the communities studied in this work. The evidence found in this study could be further used as a trigger to revisit local policies on environmental exposures.

  3. Evaluation of toxic metals in biological samples (scalp hair, blood and urine) of steel mill workers by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Afridi, Hassan I; Kazi, Tasneem G; Jamali, Mohammad K; Kazi, Gul H; Arain, Mohammad B; Jalbani, Nusrat; Shar, Ghulam Q; Sarfaraz, Raja A

    2006-10-01

    The determination of toxic metals in the biological samples of human beings is an important clinical screening procedure. This study aimed to assess the possible influence of environmental exposure on production workers (PW) and quality control workers (QCW) of a steel mill, all male subjects aged 25-55 years. In this investigation, the concentrations of Pb, Cd, Ni and Cr were determined in biological samples (blood, urine and scalp hair samples) from these steel mill workers in relation to controlled unexposed healthy subjects of the same age group. After pre-treatment with nitric acid-hydrogen peroxide, the samples were digested via a microwave oven, and for comparison purposes, the same samples were digested by the conventional wet acid digestion method. The samples digested were subjected to graphite furnace atomic absorption spectrometry (GFAAS). To assess the reliability of these methods, critical factors, such as detection limit(s), calibration range(s), accuracy and precision, were studied. Quality control for these procedures was established with certified sample of human hair, urine and whole blood. The results indicate that the level of lead, cadmium and nickel in scalp hair, blood and urine samples were significantly higher in both groups of exposed workers (QW and PW) than those of the controls. The possible connection of these elements with the etiology of disease is discussed. The results also show the need for immediate improvements in workplace ventilation and industrial hygiene practices.

  4. A Modified Protocol with Improved Detection Rate for Mis-Matched Donor HLA from Low Quantities of DNA in Urine Samples from Kidney Graft Recipients.

    Science.gov (United States)

    Kwok, Janette; Choi, Leo C W; Ho, Jenny C Y; Chan, Gavin S W; Mok, Maggie M Y; Lam, Man-Fei; Chak, Wai-Leung; Cheuk, Au; Chau, Ka-Foon; Tong, Matthew; Chan, Kwok-Wah; Chan, Tak-Mao

    2016-01-01

    Urine from kidney transplant recipient has proven to be a viable source for donor DNA. However, an optimized protocol would be required to determine mis-matched donor HLA specificities in view of the scarcity of DNA obtained in some cases. In this study, fresh early morning urine specimens were obtained from 155 kidney transplant recipients with known donor HLA phenotype. DNA was extracted and typing of HLA-A, B and DRB1 loci by polymerase chain reaction-specific sequence primers was performed using tailor-made condition according to the concentration of extracted DNA. HLA typing of DNA extracted from urine revealed both recipient and donor HLA phenotypes, allowing the deduction of the unknown donor HLA and hence the degree of HLA mis-match. By adopting the modified procedures, mis-matched donor HLA phenotypes were successfully deduced in all of 35 tested urine samples at DNA quantities spanning the range of 620-24,000 ng. This urine-based method offers a promising and reliable non-invasive means for the identification of mis-matched donor HLA antigens in kidney transplant recipients with unknown donor HLA phenotype or otherwise inadequate donor information.

  5. Mercury determination in urine samples by gold nanostructured screen-printed carbon electrodes after vortex-assisted ionic liquid dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Fernández, Elena; Vidal, Lorena; Costa-García, Agustín; Canals, Antonio

    2016-04-07

    A novel approach is presented to determine mercury in urine samples, employing vortex-assisted ionic liquid dispersive liquid-liquid microextraction and microvolume back-extraction to prepare samples, and screen-printed electrodes modified with gold nanoparticles for voltammetric analysis. Mercury was extracted directly from non-digested urine samples in a water-immiscible ionic liquid, being back-extracted into an acidic aqueous solution. Subsequently, it was determined using gold nanoparticle-modified screen-printed electrodes. Under optimized microextraction conditions, standard addition calibration was applied to urine samples containing 5, 10 and 15 μg L(-1) of mercury. Standard addition calibration curves using standards between 0 and 20 μg L(-1) gave a high level of linearity with correlation coefficients ranging from 0.990 to 0.999 (N = 5). The limit of detection was empirical and statistically evaluated, obtaining values that ranged from 0.5 to 1.5 μg L(-1), and from 1.1 to 1.3 μg L(-1), respectively, which are significantly lower than the threshold level established by the World Health Organization for normal mercury content in urine (i.e., 10-20 μg L(-1)). A certified reference material (REC-8848/Level II) was analyzed to assess method accuracy finding 87% and 3 μg L(-1) as the recovery (trueness) and standard deviation values, respectively. Finally, the method was used to analyze spiked urine samples, obtaining good agreement between spiked and found concentrations (recovery ranged from 97 to 100%).

  6. Cobas 4800 HPV detection in the cervical, vaginal and urine samples of women with high-grade CIN before and after treatment.

    Science.gov (United States)

    Stanczuk, Grazyna A; Currie, Heather; Baxter, Gwen; Foster, Adele; Gibson, Lindsay; Graham, Catriona; Cuschieri, Kate

    2015-07-01

    To assess the performance of a clinically validated human papillomavirus (HPV) test (the Cobas 4800 HPV test) in urine and self-taken vaginal specimens within a colposcopy population and to assess HPV prevalence before and after treatment across the different biospecimens. A total of 100 women attending a colposcopy clinic provided three biospecimens (a clinician-taken liquid-based cytology sample (LBC), a self-taken vaginal sample and a urine sample) for HPV testing. HPV prevalence and concordance was compared across the biospecimens and clinical performance relative to the detection of cervical intraepithelial neoplasia (CIN)2+ and CIN3+ was assessed. A total of 39 women retuned at 6 months for a post-treatment follow-up appointment, and HPV concordance in all biospecimens was measured relative to their original HPV status. 65 cases of CIN2+ were detected in the baseline population; sensitivity for CIN2+ was 92% (82 to 97) for the vaginal and the LBC sample and 80.0 (68% to 88%) for the urine sample. In the follow-up (post treatment) population, women were twice as likely to be HPV positive in their urine or vaginal sample compared with the equivalent LBC sample. Vaginal and LBC samples showed very similar performance for the detection of CIN2+ in this population using the Cobas HPV test; further validation of these findings in screening contexts will be of value. Self-taken samples may have less utility in a 'test of cure' setting-given the higher prevalence of HPV relative to LBC. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://group.bmj.com/group/rights-licensing/permissions.

  7. Comparative Study of Seven Commercial Kits for Human DNA Extraction from Urine Samples Suitable for DNA Biomarker-Based Public Health Studies

    Science.gov (United States)

    El Bali, Latifa; Diman, Aurélie; Bernard, Alfred; Roosens, Nancy H. C.; De Keersmaecker, Sigrid C. J.

    2014-01-01

    Human genomic DNA extracted from urine could be an interesting tool for large-scale public health studies involving characterization of genetic variations or DNA biomarkers as a result of the simple and noninvasive collection method. These studies, involving many samples, require a rapid, easy, and standardized extraction protocol. Moreover, for practicability, there is a necessity to collect urine at a moment different from the first void and to store it appropriately until analysis. The present study compared seven commercial kits to select the most appropriate urinary human DNA extraction procedure for epidemiological studies. DNA yield has been determined using different quantification methods: two classical, i.e., NanoDrop and PicoGreen, and two species-specific real-time quantitative (q)PCR assays, as DNA extracted from urine contains, besides human, microbial DNA also, which largely contributes to the total DNA yield. In addition, the kits giving a good yield were also tested for the presence of PCR inhibitors. Further comparisons were performed regarding the sampling time and the storage conditions. Finally, as a proof-of-concept, an important gene related to smoking has been genotyped using the developed tools. We could select one well-performing kit for the human DNA extraction from urine suitable for molecular diagnostic real-time qPCR-based assays targeting genetic variations, applicable to large-scale studies. In addition, successful genotyping was possible using DNA extracted from urine stored at −20°C for several months, and an acceptable yield could also be obtained from urine collected at different moments during the day, which is particularly important for public health studies. PMID:25365790

  8. Comparative study of seven commercial kits for human DNA extraction from urine samples suitable for DNA biomarker-based public health studies.

    Science.gov (United States)

    El Bali, Latifa; Diman, Aurélie; Bernard, Alfred; Roosens, Nancy H C; De Keersmaecker, Sigrid C J

    2014-12-01

    Human genomic DNA extracted from urine could be an interesting tool for large-scale public health studies involving characterization of genetic variations or DNA biomarkers as a result of the simple and noninvasive collection method. These studies, involving many samples, require a rapid, easy, and standardized extraction protocol. Moreover, for practicability, there is a necessity to collect urine at a moment different from the first void and to store it appropriately until analysis. The present study compared seven commercial kits to select the most appropriate urinary human DNA extraction procedure for epidemiological studies. DNA yield has been determined using different quantification methods: two classical, i.e., NanoDrop and PicoGreen, and two species-specific real-time quantitative (q)PCR assays, as DNA extracted from urine contains, besides human, microbial DNA also, which largely contributes to the total DNA yield. In addition, the kits giving a good yield were also tested for the presence of PCR inhibitors. Further comparisons were performed regarding the sampling time and the storage conditions. Finally, as a proof-of-concept, an important gene related to smoking has been genotyped using the developed tools. We could select one well-performing kit for the human DNA extraction from urine suitable for molecular diagnostic real-time qPCR-based assays targeting genetic variations, applicable to large-scale studies. In addition, successful genotyping was possible using DNA extracted from urine stored at -20°C for several months, and an acceptable yield could also be obtained from urine collected at different moments during the day, which is particularly important for public health studies.

  9. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Olmedo, P.; Pla, A.; Hernandez, A.F.; Lopez-Guarnido, O.; Rodrigo, L. [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain); Gil, F., E-mail: fgil@ugr.es [Department of Legal Medicine and Toxicology, University of Granada, School of Medicine (Spain)

    2010-02-05

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  10. Validation of a method to quantify chromium, cadmium, manganese, nickel and lead in human whole blood, urine, saliva and hair samples by electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Olmedo, P; Pla, A; Hernández, A F; López-Guarnido, O; Rodrigo, L; Gil, F

    2010-02-05

    For biological monitoring of heavy metal exposure in occupational toxicology, usually whole blood and urine samples are the most widely used and accepted matrix to assess internal xenobiotic exposure. Hair samples and saliva are also of interest in occupational and environmental health surveys but procedures for the determination of metals in saliva and hair are very scarce and to our knowledge there is no validation of a method to quantify Cr, Cd, Mn, Ni and Pb in four different human biological materials (whole blood, urine, saliva and axilary hair) by electrothermal atomization atomic absorption spectrometry (ETAAS). In the present study, quantification methods for the determination of Cr, Cd, Mn, Ni and Pb in whole blood, urine, saliva and axilary hair were validated according to the EU common standards. Pyrolisis and atomization temperatures have been determined. The main parameters evaluated were: detection and quantification limits, linearity range, repeatability, reproducibility, recovery and uncertainty. Accuracy of the methods was tested with the whole blood, urine and hair certified reference materials and recoveries of the spiked samples were acceptable ranged from 96.3 to 107.8%.

  11. Comparing capillary electrophoresis-mass spectrometry fingerprints of urine samples obtained after intake of coffee, tea, or water.

    Science.gov (United States)

    Allard, Erik; Bäckström, Daniel; Danielsson, Rolf; Sjöberg, Per J R; Bergquist, Jonas

    2008-12-01

    Metabolomic fingerprinting is a growing strategy for characterizing complex biological samples without detailed prior knowledge about the metabolic system. A two-way analysis system with liquid separation and mass spectrometric detection provides detail-rich data suitable for such fingerprints. As a model study, human urine samples, obtained after intake of coffee, tea, or water, were analyzed with capillary electrophoresis electrospray ionization time-of-flight mass spectrometry (CE-ESI-TOF-MS). In-house-developed software (in Matlab) was utilized to manage and explore the large amount of data acquired (230 CE-MS runs, each with 50-100 million nonzero data points). After baseline and noise reduction, followed by suitable binning in time and m/z, the data sets comprised 9 and 14 million data points in negative and positive ESI mode, respectively. Finally, a signal threshold was applied, further reducing the number to about 100 000 data points per data set. A set of interactive exploratory tools, utilizing principal component analysis (PCA) and analysis of variance (ANOVA) results based on a general linear model, facilitated visual interpretation with score plots (for group assessment) and differential fingerprints (for "hot spot" detection). In the model study highly significant differences due to beverage intake were obtained among the 10 first principal components (p coffee" and "tea or water" indicated several "hot spots" with highly elevated intensities (e.g., for uncharged masses 93, 94, 109, 119, 123, 132, 148, 169, 178, 187, 190, and 193) suitable for further analysis, for example, with tandem MS.

  12. Distribution of community-acquired gram negative microorganisms detected in urine samples of pediatric patients and antibiotic resistance patterns at 2013

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    Seçil Conkar

    2015-06-01

    Full Text Available Objective: This study aims to determine the antibiotic susceptibility and distribution of community-acquired microorganisms obtained from urine samples of patients admitted to our clinic in Diyarbakır, and also detect the ratio of extended spectrum beta-lactamase producing E.coli and Klebsiella strains in urine samples, and identify the antibiotics that can be used for the empiric treatment by investigating the susceptibility of extended spectrum beta-lactamase positive strains. Methods: Patients admitted to the pediatric polyclinic of our hospital between the dates 1 January-31 December were included in the study. 1167 urine samples sent to Microbiology Laboratory were examined. E.coli and Klebsiella spp. strains isolated from the urine cultures were identified with traditional methods and the Biomerium Vitek-2 compact system. Antibiotic susceptibility tests were performed in accordance with the recommendations of Clinical and Laboratory Standards Institute using Biomerium Vitek-2 compact system. Results: 959 E.coli from 1167 urine samples and other microorganisms from 26 of 182 Klebsiella spp. were isolated. Extended spectrum beta-lactamase production was detected in 445 (46.4% of E.coli strains and in 72 (39.5% of Klebsiella spp.strains. Amicasin resistance was determined as 9.4% in Extended spectrum beta-lactamase positive E.coli strains, while amicasin resistance was detected as 11% in Extended spectrum beta-lactamase positive Klebsiella spp. strains. Conclusion: Resistance development against the antibiotics has been increasingly observed in most of the microorganisms that cause urinary tract infection. We are in the opinion that this study is important for our hospital, as urinary tract infection factors vary according to centers.

  13. Determination of total iodine in serum and urine samples by ion chromatography with pulsed amperometric detection - studies on analyte loss, optimization of sample preparation procedures, and validation of analytical method.

    Science.gov (United States)

    Błażewicz, Anna; Klatka, Maria; Dolliver, Wojciech; Kocjan, Ryszard

    2014-07-01

    A fast, accurate and precise ion chromatography method with pulsed amperometric detection was applied to evaluate a variety of parameters affecting the determination of total iodine in serum and urine of 81 subjects, including 56 obese and 25 healthy Polish children. The sample pretreatment methods were carried out in a closed system and with the assistance of microwaves. Both alkaline and acidic digestion procedures were developed and optimized to find the simplest combination of reagents and the appropriate parameters for digestion that would allow for the fastest, least time consuming and most cost-effective way of analysis. A good correlation between the certified and the measured concentrations was achieved. The best recoveries (96.8% for urine and 98.8% for serum samples) were achieved using 1ml of 25% tetramethylammonium hydroxide solution within 6min for 0.1ml of serum/urine samples. Using 0.5ml of 65% nitric acid solution the best recovery (95.3%) was obtained when 7min of effective digestion time was used. Freeze-thaw stability and long-term stability were checked. After 24 weeks 14.7% loss of iodine in urine, and 10.9% in serum samples occurred. For urine samples, better correlation (R(2)=0.9891) of various sample preparation procedures (alkaline digestion and application of OnGuard RP cartidges) was obtained. Significantly lower iodide content was found in samples taken from obese children. Serum iodine content in obese children was markedly variable in comparison with the healthy group, whereas the difference was less evident when urine samples were analyzed. The mean content in serum was 59.12±8.86μg/L, and in urine 98.26±25.93 for obese children when samples were prepared by the use of optimized alkaline digestion reinforced by microwaves. In healthy children the mean content in serum was 82.58±6.01μg/L, and in urine 145.76±31.44μg/L.

  14. Automatic On-line Solid-phase Extraction-Electrothermal Atomic Absorption Spectrometry Exploiting Sequential Injection Analysis for Trace Vanadium, Cadmium and Lead Determination in Human Urine Samples.

    Science.gov (United States)

    Giakisikli, Georgia; Ayala Quezada, Alejandro; Tanaka, Junpei; Anthemidis, Aristidis N; Murakami, Hiroya; Teshima, Norio; Sakai, Tadao

    2015-01-01

    A fully automated sequential injection column preconcentration method for the on-line determination of trace vanadium, cadmium and lead in urine samples was successfully developed, utilizing electrothermal atomic absorption spectrometry (ETAAS). Polyamino-polycarboxylic acid chelating resin (Nobias chelate PA-1) packed into a handmade minicolumn was used as a sorbent material. Effective on-line retention of chelate complexes of analytes was achieved at pH 6.0, while the highest elution effectiveness was observed with 1.0 mol L(-1) HNO3 in the reverse phase. Several analytical parameters, like the sample acidity, concentration and volume of the eluent as well as the loading/elution flow rates, have been studied, regarding the efficiency of the method, providing appropriate conditions for the analysis of real samples. For a 4.5 mL sample volume, the sampling frequency was 27 h(-1). The detection limits were found to be 3.0, 0.06 and 2.0 ng L(-1) for V(V), Cd(II) and Pb(II), respectively, with the relative standard deviations ranging between 1.9 - 3.7%. The accuracy of the proposed method was evaluated by analyzing a certified reference material (Seronorm(TM) trace elements urine) and spiked urine samples.

  15. Water stable metal-organic framework packed microcolumn for online sorptive extraction and direct analysis of naproxen and its metabolite from urine sample.

    Science.gov (United States)

    Hu, Yuling; Song, Chaoyong; Liao, Jia; Huang, Zelin; Li, Gongke

    2013-06-14

    The metal-organic framework MIL-101 was fabricated in a polyetheretherketone (PEEK) tube as micro-trapping device, and applied to sorptive extraction of naproxen and its metabolite in urine samples. The remarkable water stability of the MIL-101 characterizes the material as being different from other moisture sensitive metal-organic framework. It is therefore suitable for extraction of pharmaceuticals from biological fluids. The adsorption isotherms in aqueous solution showed that the adsorption of naproxen on MIL-101 is endothermic. Additionally, MIL-101 exhibited higher extraction capacity to naproxen than that of C18-bonded silica and multi-walled nanotube. A specially designed in-tube sorptive extraction (ITSE) device endows the extraction process with the characteristic of rapidness, convenience, and easy of conjunction with high performance liquid chromatography (HPLC). Finally the MIL-101 based ITSE method coupled with HPLC and fluorescence detection was applied to analysis of naproxen and 6-O-desmethylnaproxen in urine samples. Parameters that influence the online extraction procedure, including pH of the sample solution, flow rate of extraction, sample volume, desorption solvents and time were investigated. The method is proved to be highly sensitive with the linear range of 0.05-6.0μgL(-1) and the limits of detection of 0.034 and 0.011μgL(-1) for naproxen and 6-O-desmethylnaproxen, respectively. The recoveries in urine samples were 85.3-98.3% for naproxen and 94.0-97.3% for 6-O-desmethylnaproxen with intra- and inter-day RSDs of 2.7-5.2% and 7.1-8.1%, respectively. Urine samples could be directly subjected to analysis without any additional sample pretreatment. The proposed method was demonstrated an efficient, flexible and versatile extraction tool which is ideally suitable for online conjunction with chromatographic methods.

  16. Determination Trace Levels of Vitamin C and Folic Acid in Urine Sample by Ultrasound-Assisted Dispersive Liquid-Liquid Microextraction Method Coupled HPLC-UV

    Directory of Open Access Journals (Sweden)

    Akbar Akbari

    2016-12-01

    Full Text Available A new, rapid and highly sensitive and rapid method was proposed for the simultaneous determination trace levels of vitamin C and folic acid in the human urine samples. The influence affecting factors on the UA-DLLME such as type and volume of the dispersive and extraction solvent, pH, ionic strength and temperature of sample solution, sonication condition investigated and optimized. Under the optimized extractions, relative standard deviations (RSD of the analyses less than 6% (n= 3 and detection limit of 1.65-2.05 ng mL-1 respectively. USAEME - HPLC-UV was successfully applied for the simultaneous determination of trace levels of vitamin C and folic acid in human urine Samples.

  17. Fluorescent detection of lead in environmental water and urine samples using enzyme mimics of catechin-synthesized Au nanoparticles.

    Science.gov (United States)

    Wu, Yan-Shiuan; Huang, Fan-Feng; Lin, Yang-Wei

    2013-02-01

    A facile, cost-effective, and sensitive fluorescent method for Pb²⁺ ion detection had been developed using catechin synthesized gold nanoparticles (C-Au NPs). The Pb-catechin complexes and Pb-Au alloys that formed on the C-Au NPs surfaces allowed NPs to exhibit peroxidase-mimicking catalytic activity in the H₂O₂-mediated oxidation of Amplex UltraRed (AUR). In 5 mM Tris-acetate buffers at pH 7.0, the H₂O₂-AUR-C-Au NP probe was highly selective (>100-fold) for Pb²⁺ ions in the presence of other tested metal ions (K⁺, Ag⁺, Na⁺, Cd²⁺, Ni²⁺, Ca²⁺, Hg²⁺, Sr²⁺, Co²⁺, Cu²⁺, Ba²⁺, Fe²⁺, Mg²⁺, Cr³⁺, and Fe³⁺ ions). The fluorescence intensity (excitation/emission maxima ∼540/588 nm) of the AUR product was proportional to the concentration of Pb²⁺ ions in the range of 10 nM-1.0 μM with a linear correlation (R² = 0.99). The H₂O₂-AUR-C-Au NP probe detected Pb²⁺ ions with a limit of detection (signal-to-noise ratio: 3) of 1.5 nM. The practicality of the H₂O₂-AUR-C-Au NP probe was validated for the determination of Pb²⁺ ion concentration in environmental water and urine samples, demonstrating its advantages of simplicity, selectivity, and sensitivity.

  18. [Molecular epidemiology and antifungal susceptibility of Candida species isolated from urine samples of patients in intensive care unit].

    Science.gov (United States)

    Yüksekkaya, Serife; Fındık, Duygu; Arslan, Uğur

    2011-01-01

    The aims of this study were to analyse the amphotericin B and fluconazole susceptibility and molecular epidemiology of Candida strains (Candida albicans, Candida tropicalis and Candida glabrata) isolated from the urine samples of patients hospitalized in the intensive care unit. Identification of the isolates was done according to microscopic morphology (chlamydospor, blastospor, pseudohyphae and true hyphae) on cornmeal agar, germ tube formation and carbohydrate assimilation patterns (API ID 32C bioMérieux, France). Antifungal susceptibilities of the isolates were determined by in vitro broth microdilution method recommended by Clinical and Laboratory Standards Institute (CLSI). To investigate the clonal relationship of the isolates, randomly amplified polymorphic DNA (RAPD) analysis was performed by using Cnd3 primer. Of the 56 Candida isolates minimum inhibitory concentration (MIC) ranges, MIC50 and MIC90 values for amphotericin B were 0.125-1 µg/ml, 0.125 and 0.5 µg/ml for C.albicans, 0.125-1 µg/ml, 0.25 and 1 µg/ml for C.tropicalis and 0.125-1 µg/ml, 0.25 and 1 µg/ml for C.glabrata, respectively. Fluconazole MIC ranges, MIC50 and MIC90 values were 0.25-4 µg/ml, 0.25 and 0.5 µg/ml for C.albicans, 0.25-16 µg/ml, 0.5 and 1 µg/ml for C.tropicalis and 0.5-64 µg/ml, 8 and 16 µg/ml for C.glabrata, respectively. For amphotericin B, none of the isolates had high MIC values (MIC > 1 µg/ml). While one of the C.glabrata isolates was resistant to fluconazole (MIC ≥ 64 µg/ml), one C.tropicalis and two C.glabrata isolates were dose-dependent susceptible (MIC: 16-32 µg/ml). The results of RAPD analysis indicated an exogenous spread from two clones for C.albicans, one clone for C.glabrata and one clone for C.tropicalis. This study underlines the importance of molecular epidemiological analysis of clinical samples together with hospital environmental samples in terms of Candida spp. To determine the exogenous origin for the related strains and to prevent

  19. Epidemiological investigation of the UGT2B17 polymorphism in doping control urine samples and its correlation to T/E ratios.

    Science.gov (United States)

    Anielski, Patricia; Simmchen, Juliane; Wassill, Lars; Ganghofner, Dirk; Thieme, Detlef

    2011-10-01

    The deletion polymorphism of the enzyme UGT2B17 is known to correlate with the level of the testosterone to epitestosterone (T/E) ratio in urine specimen. Due to the importance of the T/E ratio to detect testosterone abuse in doping analysis, a PCR-ELISA system (Genotype® UGT test, AmplexDiagnostics) was established to identify the UGT2B17 phenotype in urine samples. Epidemiological investigations in a set of 674 routine doping controls (in- and out-of-competition) resulted in 22.8% homozygote gene-deleted and 74.5% UGT2B17-positive athletes. The validated test system has shown to be robust and sensitive: in only 18 cases (2.7%) isolation of cell material from urine failed. Following hydrolysis of glucuronidated conjugates, steroids were analyzed as bis-TMS derivatives by gas chromatography-mass spectrometry (GC-MS), for example, testosterone (T) and epitestosterone (E). Additionally, isotope ration mass spectrometry (IRMS) analysis and luteinizing hormone (LH) measurement were applied. Mean T/E ratios significantly correlated with the UGT2B17 phenotype (del: T/E 0.9; pos: 1.7), however the values did not differ as distinctive as reported in previous studies. Additionally, the T/E ratios in the gene-deleted group did not show a normal curve of distribution (median of T/E 0.5). Obviously, beside the UGT2B17 deletion further influences have to be taken into account, for example, polymorphisms or induction of other metabolizing enzymes. Our results indicate that the UGT2B17 polymorphism might be insufficient when utilized solely as a crucial parameter for individual interpretation of T/E in urine. Nevertheless, the detection of the UGT2B17-gene deletion in urine samples would provide additional information important for gathering evidence in analysis of steroids in doping control.

  20. A sensitive determination of terbutaline in pharmaceuticals and urine samples using a composite electrode based on zirconium oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet, E-mail: maslanoglu@harran.edu.tr

    2016-10-01

    An accurate and precise determination of terbutaline has been carried out using a glassy carbon electrode (GCE) modified with a composite of multi-walled carbon nanotubes (MWCNTs) and nanoparticles of zirconium oxide (ZrO{sub 2}NPs). Energy dispersive X-ray and scanning electron microscopic techniques were utilized for the characterization of the composite layer. Terbutaline exhibited a broad oxidation peak at 770 mV on a GCE. However, MWCNTs/GCE presented an electrocatalytic effect toward the oxidation of terbutaline with a better anodic peak at 660 mV. Furthermore, the electrochemical behavior of terbutaline has greatly been improved at a GCE modified with a composite of MWCNTs and nanoparticles of ZrO{sub 2}. The ZrO{sub 2}NPs/MWCNTs/GCE exhibited a sharp anodic wave at 645 mV with a large enhancement of the current response for terbutaline. Square wave voltammetry (SWV) was performed for the determination of terbutaline at ZrO{sub 2}NPs/MWCNTs/GCE. A linear plot was obtained for the current responses of terbutaline against concentrations in the range of 10–160 nM yielding a detection limit of 2.25 nM (based on 3S{sub b}/m). Improved voltammetric behavior, long-time stability and good reproducibility were obtained for terbutaline at the proposed electrode. A mean recovery of 101.2% with an RSD% of 1.9 was obtained for the analysis of the drug formulation. The accurate and precise quantification of terbutaline makes the ZrO{sub 2}NPs/MWCNTs/GCE system of great interest for monitoring its therapeutic use. - Graphical abstract: A sensitive determination of terbutaline in pharmaceuticals and urine samples using a composite electrode based on zirconium oxide nanoparticles. Display Omitted - Highlights: • A composite electrode was prepared using nanoparticles of ZrO{sub 2} and MWCNTs. • The ZrO{sub 2}NPs/MWCNTs/GCE has greatly improved the voltammetry of terbutaline • The proposed electrode enabled a detection limit of 2.25 nM. • The proposed electrode

  1. Automated extraction of 11-nor-delta9-tetrahydrocannabinol carboxylic acid from urine samples using the ASPEC XL solid-phase extraction system.

    Science.gov (United States)

    Langen, M C; de Bijl, G A; Egberts, A C

    2000-09-01

    The analysis of 11-nor-delta9-tetrahydrocannabinol-carboxylic acid (THCCOOH, the major metabolite of cannabis) in urine with gas chromatography and mass spectrometry (GC-MS) and solid-phase extraction (SPE) sample preparation is well documented. Automated SPE sample preparation of THCCOOH in urine, although potentially advantageous, is to our knowledge poorly investigated. The objective of the present study was to develop and validate an automated SPE sample-preparation step using ASPEC XL suited for GC-MS confirmation analysis of THCCOOH in urine drug control. The recoveries showed that it was not possible to transfer the protocol for the manual SPE procedure with the vacuum manifold to the ASPEC XL without loss of recovery. Making the sample more lipophilic by adding 1 mL 2-propanol after hydrolysis to the urine sample in order to overcome the problem of surface adsorption of THCCOOH led to an extraction efficiency (77%) comparable to that reached with the vacuum manifold (84%). The reproducibility of the automated SPE procedure was better (coefficient of variation 5%) than that of the manual procedure (coefficient of variation 12%). The limit of detection was 1 ng/mL, and the limit of quantitation was 4 ng/mL. Precision at the 12.5-ng/mL level was as follows: mean, 12.4 and coefficient of variation, 3.0%. Potential carryover was evaluated, but a carryover effect could not be detected. It was concluded that the proposed method is suited for GC-MS confirmation urinalysis of THCCOOH for prisons and detoxification centers.

  2. Copper nanowires immobilized on the boards of microfluidic chips for the rapid and simultaneous diagnosis of galactosemia diseases in newborn urine samples.

    Science.gov (United States)

    García, Miguel; Alonso-Fernández, José Ramón; Escarpa, Alberto

    2013-10-01

    Galactosemia is a rare disease that is diagnosed through the identification of different metabolite profiles. Therefore, the specific detection of galactose 1-phosphate (Gal 1-P), galactose (Gal), and uridyl diphosphate galactose (UDP-Gal) confirms type I, II, and III galactosemia diseases. Because of the low prevalence of galactosemia, sample availability is very scarce and screening methods to diagnose the illness are not commonly employed around the world. This work describes the coupling of microfluidic chips (MCs) to copper nanowires (CuNWs) as electrochemical detectors for the fast diagnosis of galactosemia in precious newborn urine samples. Conceptually speaking, we hypothesize that the inherent selectivity and sensitivity of CuNWs, toward galactosemia metabolites detection in connection with MC selectivity could allow the fast and simultaneous detection of the three galactosemia biomarkers, which implies the fast diagnosis of any galactosemia type in just one single analysis. Electrosynthesized CuNWs show a well-defined shape, with an average length of 6 μm and a width of 300 nm. The modified electrodes exhibited an enhanced electroactive surface area twice as high as the nonmodified ones. Very good intraelectrode repeatability with relative standard deviations (RSDs) of galactosemia diseases were unequivocally identified, differentiating between type I, II, and III, using selected precious ill diagnosed newborn urine samples. Detection proceeded within less than 350 s, required negligible urine sample consumption, and displayed impressive signal-to-noise characteristics (ranging from 14 to 80) and micromolar limits of detection (LODs) much lower than the cutoff levels (Gal 1-P > 0.4 mM and Gal > 1.4 mM). Excellent reproducible recoveries (93%-107%, RSDs <6%) were also achieved, revealing the reliability of the approach. The significance of the newborn urine samples studied confirms the analytical potency of MC-CuNWs approach, enhancing the maturity of the

  3. Poly(methacrylic acid-ethylene glycol dimethacrylate) monolith in-tube solid phase microextraction coupled to high performance liquid chromatography and analysis of amphetamines in urine samples.

    Science.gov (United States)

    Fan, Yi; Feng, Yu-Qi; Zhang, Jian-Tao; Da, Shi-Lu; Zhang, Min

    2005-05-13

    In-tube solid-phase microextraction (SPME) based on a poly(methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was investigated for the extraction of amphetamine, methamphetamine and their methylenedioxy derivatives. The monolithic capillary column showed high extraction efficiency towards target analytes, which could be attributed to its larger loading amount of extraction phase than conventional open-tubular extraction capillaries and the convective mass transfer procedure provided by its monolithic structure. The extraction mechanism was studied, and the results indicated that the extraction process of the target analytes was involved with hydrophobic interaction and ion-exchange interaction. The polymer monolith in-tube SPME-HPLC system with UV detection was successfully applied to the determination of amphetamine, methamphetamine and their methylenedioxy derivatives in urine samples, yielding the detection limits of 1.4 - 4.0 ng/mL. Excellent method reproducibility (RSD urine samples.

  4. Myoglobin urine test

    Science.gov (United States)

    Urine myoglobin; Heart attack - myoglobin urine test; Myositis - myoglobin urine test; Rhabdomyolysis - myoglobin urine test ... The test involves only normal urination, which should cause no discomfort.

  5. Emergency Radiobioassay Method for Determination of ⁹⁰Sr and ²²⁶Ra in a Spot Urine Sample.

    Science.gov (United States)

    Sadi, Baki B; Fontaine, Allison; McAlister, Daniel; Li, Chunsheng

    2015-08-04

    A new radiobioassay method has been developed for simultaneous determination of (90)Sr and (226)Ra in a spot urine sample. The method is based on a matrix removal procedure to purify the target radionuclides from a urine sample followed by an automated high performance ion chromatographic (HPIC) separation of (90)Sr and (226)Ra and offline radiometric detection by liquid scintillation counting (LSC). A Sr-resin extraction chromatographic cartridge was used for matrix removal and purification of (90)Sr and (226)Ra from a urine sample prior to its introduction to the HPIC system. The HPIC separation was carried out through cation exchange chromatography using methanesulfonic acid (75 mM) as the mobile phase at 0.25 mL/min flow rate. The performance criteria of the method was evaluated against the American National Standard Institute ANSI/HPS N13.30-2011 standard for the root mean squared error (RMSE) of relative bias (Br) and relative precision (SB) at two different spiked activity levels. The RMSE of Br and SB for (90)Sr and (226)Ra were found to be satisfactory (≤0.25). The minimum detectable activity (MDA) of the method for (90)Sr and (226)Ra are 2 Bq/L and 0.2 Bq/L, respectively. The MDA values are at least 1/10th of the concentrations of (90)Sr (190 Bq/L) and (226)Ra (2 Bq/L) excreted in urine on the third day following an acute exposure (inhalation) that would lead to an effective dose of 0.1 Sv in the first year. The sample turnaround time is less than 8 h for simultaneous determination of (90)Sr and (226)Ra.

  6. Diagnostic accuracy and applicability of a PCR system for the detection of Schistosoma mansoni DNA in human urine samples from an endemic area.

    Directory of Open Access Journals (Sweden)

    Martin Johannes Enk

    Full Text Available Schistosomiasis caused by Schistosoma mansoni, one of the most neglected human parasitoses in Latin America and Africa, is routinely confirmed by microscopic visualization of eggs in stool. The main limitation of this diagnostic approach is its lack of sensitivity in detecting individual low worm burdens and consequently data on infection rates in low transmission settings are little reliable. According to the scientific literature, PCR assays are characterized by high sensitivity and specificity in detecting parasite DNA in biological samples. A simple and cost effective extraction method for DNA of Schistosoma mansoni from urine samples in combination with a conventional PCR assay was developed and applied in an endemic area. This urine based PCR system was tested for diagnostic accuracy among a population of a small village in an endemic area, comparing it to a reference test composed of three different parasitological techniques. The diagnostic parameters revealed a sensitivity of 100%, a specificity of 91.20%, positive and negative predictive values of 86.25% and 100%, respectively, and a test accuracy of 94.33%. Further statistical analysis showed a k index of 0.8806, indicating an excellent agreement between the reference test and the PCR system. Data obtained from the mouse model indicate the infection can be detected one week after cercariae penetration, opening a new perspective for early detection and patient management during this stage of the disease. The data indicate that this innovative PCR system provides a simple to handle and robust diagnostic tool for the detection of S. mansoni DNA from urine samples and a promising approach to overcome the diagnostic obstacles in low transmission settings. Furthermore the principals of this molecular technique, based on the examination of human urine samples may be useful for the diagnosis of other neglected tropical diseases that can be detected by trans-renal DNA.

  7. Dual-cloud point extraction coupled to high performance liquid chromatography for simultaneous determination of trace sulfonamide antimicrobials in urine and water samples.

    Science.gov (United States)

    Nong, Chunyan; Niu, Zongliang; Li, Pengyao; Wang, Chunping; Li, Wanyu; Wen, Yingying

    2017-03-01

    Dual-cloud point extraction (dCPE) was successfully developed for simultaneous extraction of trace sulfonamides (SAs) including sulfamerazine (SMZ), sulfadoxin (SDX), sulfathiazole (STZ) in urine and water samples. Several parameters affecting the extraction were optimized, such as sample pH, concentration of Triton X-114, extraction temperature and time, centrifugation rate and time, back-extraction solution pH, back-extraction temperature and time, back-extraction centrifugation rate and time. High performance liquid chromatography (HPLC) was applied for the SAs analysis. Under the optimum extraction and detection conditions, successful separation of the SAs was achieved within 9min, and excellent analytical performances were attained. Good linear relationships (R(2)≥0.9990) between peak area and concentration for SMZ and STZ were optimized from 0.02 to 10μg/mL, for SDX from 0.01 to 10μg/mL. Detection limits of 3.0-6.2ng/mL were achieved. Satisfactory recoveries ranging from 85 to 108% were determined with urine, lake and tap water spiked at 0.2, 0.5 and 1μg/mL, respectively, with relative standard deviations (RSDs, n=6) of 1.5-7.7%. This method was demonstrated to be convenient, rapid, cost-effective and environmentally benign, and could be used as an alternative tool to existing methods for analysing trace residues of SAs in urine and water samples.

  8. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples.

    Science.gov (United States)

    Yang, Jiajia; Li, Yun; Wang, Jincheng; Sun, Xiaoli; Cao, Rong; Sun, Hao; Huang, Chaonan; Chen, Jiping

    2015-05-01

    The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30-60 μm), a specific surface area (S(BET)) of 281.26 m(2) g(-1) and a total pore volume (V(t)) of 0.459 cm(3) g(-1). Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2-2.2 ng mL(-1). The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL(-1) for each BP) were in the range of 81.3-106.7% with RSD values below 8.3%.

  9. Carbon coated magnetic nanoparticles as a novel magnetic solid phase extraction adsorbent for simultaneous extraction of methamphetamine and ephedrine from urine samples.

    Science.gov (United States)

    Taghvimi, Arezou; Hamishehkar, Hamed

    2017-01-15

    This paper develops a highly selective, specific and efficient method for simultaneous determination of ephedrine and methamphetamine by a new carbon coated magnetic nanoparticles (C/MNPs) as a magnetic solid phase extraction (MSPE) adsorbent in biological urine medium. The characterization of synthesized magnetic nano adsorbent was completely carried out by various characterization techniques like Fourier transform infrared (FT-IR) spectroscopy, powder x-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). Nine important parameters influencing extraction efficiency including amount of adsorbent, amounts of sample volume, pH, type and amount of extraction organic solvent, time of extraction and desorption, agitation rate and ionic strength of extraction medium, were studied and optimized. Under optimized extraction conditions, a good linearity was observed in the concentration range of 100-2000ng/mL for ephedrine and 100-2500ng/mL for methamphetamine. Analysis of positive urine samples was carried out by proposed method with the recovery of 98.71 and 97.87% for ephedrine and methamphetamine, respectively. The results indicated that carbon coated magnetic nanoparticles could be applied in clinical and forensic laboratories for simultaneous determination of abused drugs in urine media.

  10. Optimization and clinical validation of a Real-Time PCR protocol for direct detection of Trichomonas vaginalis in pooled urine samples

    Directory of Open Access Journals (Sweden)

    WHA Zandijk

    2009-12-01

    Full Text Available Background and Objectives: A new Real- Time PCR protocol for the detection of Trichomonas vaginalis in pooled urine"nsamples has been optimized and validated."nMaterials and Methods: The amplification protocol, targeting a 2kb repeated gene in the T. vaginalis genome, was optimized"nby varying PCR parameters. As a reference method, a Real-Time PCR protocol targeting the beta-tubulin gene (Y. Versluis"net al, 2006, Int J STD AIDS 17:642 was used. Clinical validation was performed with pooled urine samples obtained from"npatients of the sexually transmitted diseases clinic of a university hospital (n=963; from February – June 2007."nResults: Positive samples with the new optimized technique is 1.1% (n=10, while the beta-tubulin real-time PCR method"ngenerated four positives (0.3%."nConclusion: The new RT- PCR protocol is a sensitive (1.000 and specific (0.993 procedure to detect and to identify T."nvaginalis in urine samples.

  11. Molecularly imprinted polymer in microextraction by packed sorbent for the simultaneous determination of local anesthetics: lidocaine, ropivacaine, mepivacaine and bupivacaine in plasma and urine samples.

    Science.gov (United States)

    Daryanavard, Seyed Mosayeb; Jeppsson-Dadoun, Amin; Andersson, Lars I; Hashemi, Mahdi; Colmsjö, Anders; Abdel-Rehim, Mohamed

    2013-11-01

    This study presents the use of molecularly imprinted polymer (MIP) as packing material for microextraction by packed syringe (MEPS) to achieve higher extraction selectivity. Pentycaine was used as template for MIP. Development and validation of the determination of lidocaine, ropivacaine, mepivacaine and bupivacaine in human plasma and urine samples utilizing MIP-MEPS and liquid chromatography-tandem mass spectrometry (LC-MS/MS) were carried out. The MEPS MIP-cartridge could be used for 100 extractions before it was discarded. The extraction recovery ranged from 60 to 80%. The correlation coefficients values were >0.999 for all assays using lidocaine, ropivacaine, mepivacaine and bupivacaine in the calibration range 5-2000 nmol/L. The accuracy of the studied compounds, given as a percentage variation from the nominal concentration values, ranged from -4.9 to 8.4% using plasma and urine samples. The between-batch precision, given as the relative standard deviation, at three different concentrations (quality control samples) was ranged from -4.7 to 14.0% and from 1.8 to 12.7% in plasma and urine, respectively. The lower limit of quantification and limit of detection of the studied substances were 5.0 and 1.0 nm, respectively. Copyright © 2013 John Wiley & Sons, Ltd.

  12. Combination of counter current salting-out homogenous liquid-liquid extraction and dispersive liquid-liquid microextraction as a novel microextraction of drugs in urine samples.

    Science.gov (United States)

    Akramipour, Reza; Fattahi, Nazir; Pirsaheb, Meghdad; Gheini, Simin

    2016-02-15

    The counter current salting-out homogenous liquid-liquid extraction (CCSHLLE) joined with the dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) has been developed as a high preconcentration technique for the determination of different drugs in urine samples. Amphetamines were employed as model compounds to assess the extraction procedure and were determined by high performance liquid chromatography-ultraviolet detection (HPLC-UV). In this method, initially, NaCl as a separation reagent is filled into a small column and a mixture of urine and acetonitrile is passed through the column. By passing the mixture, NaCl is dissolved and the fine droplets of acetonitrile are formed due to salting-out effect. The produced droplets go up through the remained mixture and collect as a separated layer. Then, the collected acetonitrile is removed with a syringe and mixed with 30.0μL 1-undecanol (extraction solvent). In the second step, the 5.00mLK2CO3 solution (2% w/v) is rapidly injected into the above mixture placed in a test tube for further DLLME-SFO. Under the optimum conditions, calibration curves are linear in the range of 1-3000μgL(-1) and limit of detections (LODs) are in the range of 0.5-2μgL(-1). The extraction recoveries and enrichment factors ranged from 78 to 84% and 157 to 168, respectively. Repeatability (intra-day) and reproducibility (inter-day) of method based on seven replicate measurements of 100μgL(-1) of amphetamines were in the range of 3.5-4.5% and 4-5%, respectively. The method was successfully applied for the determination of amphetamines in the actual urine samples. The relative recoveries of urine samples spiked with amphetamine and methamphetamine are 90-108%.

  13. Validity of protein-osmolality versus protein-creatinine ratios in the estimation of quantitative proteinuria from random samples of urine in children.

    Science.gov (United States)

    Morgenstern, Bruce Z; Butani, Lavjay; Wollan, Peter; Wilson, David M; Larson, Timothy S

    2003-04-01

    Proteinuria is an important marker of kidney disease. Simple methods to determine the presence of proteinuria in a semiquantitative fashion require measurement of either a protein-creatinine or protein-osmolality ratio. Urine samples from 134 healthy infants and children and 150 children from the pediatric nephrology practice were analyzed to develop normative data for protein-osmolality ratios on random urine samples and compare protein-osmolality with protein-creatinine ratio as a predictor of 24-hour urine protein excretion. Children were grouped according to age. Three groups were established: infants (<2 years), younger children (2 to 8 years), and older children (9 to 18 years). An adult cohort was similarly analyzed. For healthy children older than 2 years, the optimal value discriminating normal from abnormal protein excretion was determined to be a protein-osmolality ratio of 0.15 mg x kg H2O/mOsm. L; for children between 2 and 8 years old, 0.14; and for children older than 8 years, 0.17 (P = not significant between age groups). The corresponding optimal cutoff value for protein-creatinine ratio for the entire group of children older than 2 years is 0.20. Area under the curve analysis of receiver operator characteristic curves showed protein-creatinine ratio was superior to protein-osmolality ratio for predicting abnormal amounts of proteinuria in children and adolescents (P < 0.0001). In adults, both ratios are equally accurate. Given the superiority of protein-creatinine ratio in children, it would be appropriate to screen urine samples for proteinuria using protein-creatinine ratio rather than protein-osmolality ratio.

  14. Analytical sample preparation strategies for the determination of antimalarial drugs in human whole blood, plasma and urine

    DEFF Research Database (Denmark)

    Casas, Monica Escolà; Hansen, Martin; Krogh, Kristine A;

    2014-01-01

    Antimalarial drugs commonly referred to as antimalarials, include a variety of compounds with different physicochemical properties. There is a lack of information on antimalarial distribution in the body over time after administration, e.g. the drug concentrations in whole blood, plasma, and urin...... summarized. Finally, the main problems that the researchers have dealt with are highlighted. This information will aid analytical chemists in the development of novel methods for determining existing antimalarials and upcoming new drugs.......Antimalarial drugs commonly referred to as antimalarials, include a variety of compounds with different physicochemical properties. There is a lack of information on antimalarial distribution in the body over time after administration, e.g. the drug concentrations in whole blood, plasma, and urine...

  15. Confirmatory method for the determination of resorcylic acid lactones in urine sample using immunoaffinity cleanup and liquid chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dusi, Guglielmo [Istituto Zooprofilattico Sperimentale della Lombardia e dell' Emilia Romagna, ' B. Ubertini' , Via Bianchi 7, 25124 Brescia (Italy)], E-mail: guglielmo.dusi@bs.izs.it; Bozzoni, Eros; Assini, Walter; Tognoli, Nadia; Gasparini, Mara; Ferretti, Enrica [Istituto Zooprofilattico Sperimentale della Lombardia e dell' Emilia Romagna, ' B. Ubertini' , Via Bianchi 7, 25124 Brescia (Italy)

    2009-04-01

    The presence of zeranol ({alpha}-zearalanol) in urine samples due to natural contamination or illegal treatment is under debate within the European Union. The simultaneous determination of zeranol, its epimer taleranol ({beta}-zearalanol), zearalanone and the structurally related mycotoxin zearalenone with the corresponding {alpha}- and {beta}-zearalenol metabolites appears to be critical in deciding whether an illegal use has occurred. The aim of this study is to develop and validate a simple analytical procedure applicable to bovine and swine urine samples for the determination of all six resorcylic acid lactones. After an enzymatic deconjugation, the urine was subjected to a one-step cleanup on a commercially available immunoaffinity chromatography cartridge. The analytes were detected by liquid chromatography-negative-ion electrospray tandem mass spectrometry using deuterium-labelled internal standards. The method was validated as a quantitative confirmatory method according to European Commission Decision 2002/657/EC. The evaluated parameters were: linearity, specificity, precision (repeatability and intra-laboratory reproducibility), recovery, decision limit, detection capability and ruggedness. The decision limits (CC{alpha}) obtained, were between 0.56 and 0.68 {mu}g L{sup -1}; recovery above 66% for all the analytes. Repeatability was between 1.4 and 5.3% and within-laboratory reproducibility between 1.9 and 16.1% for the six resorcylic acid lactones.

  16. Extraction of benzoylecgonine (cocaine metabolite) and opiates (codeine and morphine) from urine samples using the Zymark RapidTrace.

    Science.gov (United States)

    Diamond, F X; Vickery, W E; de Kanel, J

    1996-01-01

    The Zymark RapidTrace automated solid-phase extraction system has been evaluated for use in the urine drug-testing laboratory. Methods for cocaine metabolite (benzoylecgonine) and opiates (codeine and morphine) are described and evaluated. The linearity, precision, accuracy, recovery, and carryover statistics of these analytical protocols are presented. The advantages of extraction using the RapidTrace instead of solid-phase extraction with the manual vacuum manifold or liquid-liquid extraction methods are described.

  17. Simultaneous determination of cefotaxime and desacetylcefotaxime in real urine sample using voltammetric and high-performance liquid chromatographic methods.

    Science.gov (United States)

    Aleksić, Mara M; Kapetanović, Vera; Atanacković, Jasmina; Jocić, Biljana; Zecević, Mira

    2008-10-19

    Two rapid, accurate and sensitive methods are developed and validated for the quantitative simultaneous determination of cefotaxime (CFX) and its active metabolite desacetylcefotaxime (DCFX) in urine. Based on the previous results which showed the four electron reduction of CFX at approximately -0.5 V, and the new findings that DCFX reduction occurred at more positive potential (-0.23 V), the new adsorptive stripping differential pulse voltammetric (AdSDPV) method was developed for determination of CFX in the presence of DCFX. Linear responses were observed over a wide concentration range (0.07-0.52 microg/ml for CFX and 0.22-1.3 microg/ml for DCFX) in urine. The second assay involves subsequent separation on a reversed-phase HPLC column, with ultraviolet detection at 262 nm. Retention times were 4.057 and 1.960 min for CFX and DCFX, respectively. Linear responses were observed over a wide range, 0.55-6.60 microg/ml for CFX and 1.10-11.00 microg/ml for DCFX, in urine. The statistical evaluation for both methods was examined by means of within-day repeatability (n=5) and day-to-day precision (n=3) and was found to be satisfactory with high accuracy and precision.

  18. Simultaneous extraction and quantification of lamotrigine, phenobarbital, and phenytoin in human plasma and urine samples using solidified floating organic drop microextraction and high-performance liquid chromatography.

    Science.gov (United States)

    Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Abbasi, Bijan

    2015-07-01

    A novel and simple method based on solidified floating organic drop microextraction followed by high-performance liquid chromatography with ultraviolet detection has been developed for simultaneous preconcentration and determination of phenobarbital, lamotrigine, and phenytoin in human plasma and urine samples. Factors affecting microextraction efficiency such as the type and volume of the extraction solvent, sample pH, extraction time, stirring rate, extraction temperature, ionic strength, and sample volume were optimized. Under the optimum conditions (i.e. extraction solvent, 1-undecanol (40 μL); sample pH, 8.0; temperature, 25°C; stirring rate, 500 rpm; sample volume, 7 mL; potassium chloride concentration, 5% and extraction time, 50 min), the limits of detection for phenobarbital, lamotrigine, and phenytoin were 1.0, 0.1, and 0.3 μg/L, respectively. Also, the calibration curves for phenobarbital, lamotrigine, and phenytoin were linear in the concentration range of 2.0-300.0, 0.3-200.0, and 1.0-200.0 μg/L, respectively. The relative standard deviations for six replicate extractions and determinations of phenobarbital, lamotrigine, and phenytoin at 50 μg/L level were less than 4.6%. The method was successfully applied to determine phenobarbital, lamotrigine, and phenytoin in plasma and urine samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Evaluation of status of trace and toxic metals in biological samples (scalp hair, blood, and urine) of normal and anemic children of two age groups.

    Science.gov (United States)

    Shah, Faheem; Kazi, Tasneem Gul; Afridi, Hassan Imran; Kazi, Naveed; Baig, Jameel Ahmed; Shah, Abdul Qadir; Khan, Sumaira; Kolachi, Nida Fatima; Wadhwa, Sham Kumar

    2011-06-01

    Anemia affects a substantial portion of the world's population, provoking severe health problems as well as important economic losses to the region in which this condition is found. This study was designed to compare the levels of essential trace and toxic elements in scalp hair, blood, and urine samples of anemic children (n = 132) with age range 1-5 and 6-10 years of both genders. For a comparative study, 134 non-anemic age- and sex-matched children as control subjects, residing in the same city, were selected. The metals in the biological samples were measured by flame atomic absorption spectrophotometry/electrothermal atomic absorption spectrometry prior to microwave-assisted acid digestion. The proposed method was validated using certified reference samples of hair, blood, and urine. The results indicated significantly lower levels of iron, copper, and zinc in the biological samples as compared to the control children of both genders (p = 0.01-0.008). The mean values of lead and cadmium were significantly high in all three biological samples of anemic children as compared to non-anemic children of both age groups (p = 0.005-0.001). The ratios of essential metal to toxic metals in the biological samples of anemic children of both age groups were significantly lower than that of controls. Deficiency of essential trace metals and high level of toxic metals may play a role in the development of anemia in the subjects under study.

  20. Simultaneous quantification of four metabolites of sulfur mustard in urine samples by ultra-high performance liquid chromatography-tandem mass spectrometry after solid phase extraction.

    Science.gov (United States)

    Liu, Chang-Cai; Liu, Shi-Lei; Xi, Hai-Ling; Yu, Hui-Lan; Zhou, Shi-Kun; Huang, Gui-Lan; Liang, Long-Hui; Liu, Jing-Quan

    2017-04-07

    Four HD urinary metabolites including hydrolysis metabolite thiodiglycol (TDG), glutathione-derived metabolite 1,1'-sulfonylbis[2-S-(N-acetylcysteinyl)ethane] (SBSNAE), as well as the β-lyase metabolites 1,1'-sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE) and 1-methylsulfinyl-2-[2-(methylthio) ethylsulfonyl]ethane (MSMTESE) are considered as important biomarkers for short-term retrospective detection of HD exposure. In this study, a single method for simultaneous quantification of the four HD metabolites in urine samples was developed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The four urinary metabolites were simultaneously extracted from urinary samples using a solid phase extraction (SPE) method with high extraction recoveries for all four metabolites varied in the range of 71.1-103% followed by UHPLC-MS/MS analysis. The SPE is simple and high effective only requiring 0.1mL of urinary samples and 0.5h time consuming. The problem of previous co-elution of TDG and SBSNAE in UHPLC was well solved, and complete separation of TDG, SBSNAE, SBMSE and MSMTESE from SPE-processed urine matrix was obtained to increase specificity and sensitivity. A full method validation was performed for each analyte in urine matrix. The linear range of calibration curves for the four analytes were respectively from 0.50-500ngmL(-1) for TDG and SBSNAE, 0.05-500ngmL(-1) for SBMSE and MSMTESE with coefficient of determination value (R(2)) ≥0.990. The limit of detection was 0.25ngmL(-1) for TDG and SBSNAE, 0.01ngmL(-1) for SBMSE and MSMTESE spiked in normal urine. The intra/inter-day precision for each analyte at three QC levels had relative standard deviation (%RSD) of ≤10.3%, and the intra/inter-day accuracy ranged between 88.0-108%. This developed method allows for simultaneous and trace measurement of four HD urinary metabolites within one single determination with the lowest usage amount of urine samples over all previous methods This

  1. Identification and quantification of flavonoids in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Freese, R.; Cornett, C.

    2000-01-01

    A rapid and sensitive high-performance liquid chromatographic mass spectrometric (HPLC-MS) method is described for the determination and quantification of 12 dietary flavonoid glycosides and aglycons in human urine samples. Chromatographic separation of the analytes of interest was achieved...... by column-switching, using the first column (a Zorbax 300SB C-3 column) for sample cleanup and eluting the heart-cut flavonoid fraction onto the second column (a Zorbax SE C-18 column) for separation and detection by ultraviolet and atmospheric pressure chemical ionization MS using single ion monitoring...... with high and low flavonoid content was analyzed, and the results are reported....

  2. Perfiles genéticos en muestras de orina en identificación sanitaria militar Genetic profiles in urine samples in military medical identification

    Directory of Open Access Journals (Sweden)

    M.L. Marqués Negredo

    2012-06-01

    Full Text Available Antecedentes: Las muestras de orina que con frecuencia son utilizadas para análisis clínicos, toxicológicos o tets de control de dopaje, pueden verse mezcladas de forma inconsciente o manipuladas intencionalmente. Objetivos: Disponer de una técnica que permita asegurar la identidad de las muestras de orina. Se propone la identificación del donante a partir de la comparación de perfiles genéticos en muestras de orina y sangre. Comparamos dos métodos de extracción de DNA nuclear. Material y métodos: Extracción de DNA a partir de dos métodos, el protocolo Master Diagnostica (VITRO, S.A. y el método automático MagNa Pure® de Roche. Se establece los perfiles genéticos según el AmpFlSTR® Identifiler® PCR Amplification Kit (Applied Biosystems. Resultados: Se obtuvo 100 % de concordancias entre los perfiles de los dos tipos de muestras. Conclusiones: Tanto de forma manual como automática se puede obtener DNA a partir de muestras de orina. Ambos métodos son válidos, si bien con el manual, se obtiene mayor cantidad de DNA. Se puede identificar al donante de una muestra de orina comparando los perfiles genéticos de la orina y de la sangre. La extracción del DNA de la orina y su posterior almacenamiento a -80ºC permite el establecimiento del perfil genético a posteriori sin alteraciones.Antecedents: Urine samples that are often utilized for clinical, toxicological or doping control tests can be mistaken involuntarily or intentionally tampered with. Objective: To make available a technique that ensures the identity of urine samples. We propose the identification of the donor through genetic profiling in blood and urine samples. Two methods of nuclear DNA extraction are compared. Material and methods: DNA is extracted by two methods, the method of Master Diagnostica (VITRO S.A. and the automatic method MagNa Pure® of Roche. The genetic profiles are established utilizing the AmpFlSTR® Identifiler® PCR Amplification Kit (Applied

  3. [Preparation of molecularly imprinted polymers using dummy template and the applications in selective solid-phase extraction of seven bisphenols from human urine, bovine serum and beer samples].

    Science.gov (United States)

    Yang, Jiajia; Li, Yun; Wang Jinchengt; Sun, Xiaoli; Chen, Jiping

    2015-05-01

    A molecularly imprinted polymer (MIP) for selective recognition of seven bisphenols (BPs) was prepared using dummy template phenolphthalein (PP) by bulk polymerization. The characterization results of scanning electron microscopy and nitrogen adsorption-desorption measurements showed that the prepared PP-MIP possessed narrow particle diameter distribution (40-60 µm), a specific surface area (S(BET)) of 359.77 m2/g and a total pore volume (Vt) of 0.730 cm3/g. The adsorption capacity for bisphenol A (BPA) of PP-MIP was evaluated by static adsorption experiment. And the Scatchard analysis revealed that the maximum specific adsorption capacity of PP-MIP was 4.661 µmol/g. Good class selectivity for BPA and its six structural analogues of bisphenol B (BPB) , bisphenol E (BPE), bisphenol AF (BPAF), bisphenol S (BPS), bisphenol AP (BPAP) and bisphenol Z (BPZ) was demonstrated by the chromatographic evaluation experiment. The prepared PP-MIP was successfully used as solid-phase extraction (SPE) sorbent for the separation and purification of the seven BPs in human urine, bovine serum and beer samples. Meanwhile, an accurate and sensitive MIP-SPE-HPLC method was established for the determination of the seven BPs in human urine, bovine serum and beer samples. The limits of detection (LODs) for the three samples were in the range of 1.2-2.0 µg/L. The results showed that good linearities were obtained in the range of 0.02-2 mg/L for the seven BPs and the correlation coefficients (r) were higher than 0.999 8. The recoveries of the BPs spiked in blank samples at two spiked levels (100 and 500 µg/L for each BP) were in the range of 90.1%-107.1% with the RSDs ≤ 8.1%. The proposed method is simple and reliable for the rapid detection of the seven BPs in human urine, bovine serum and beer samples.

  4. Reassessment of 239Pu on planchets from human urine samples at ultra-trace levels using Aridus-ICPSFMS and AMS.

    Science.gov (United States)

    Hernández-Mendoza, Héctor; Chamizo, Elena; Delgado, Antonio; García-León, Manuel; Yllera, Abel

    2012-12-01

    New analytical methods developed at the facilities here, based on two ultra-sensitive mass spectrometry (MS) techniques, inductively coupled plasma sector field mass spectrometer with a desolvator system (Aridus-ICP-SFMS) and accelerator MS (AMS), have been applied in this work for the reassessment of (239)Pu in alpha spectrometry (AS) planchets corresponding to spiked human urine samples. The obtained (239)Pu minimum detectable activities (MDAs) values by Aridus-ICP-SFMS and AMS were 3 fg (∼6.92 µBq) and 0.4 fg (∼0.92 µBq), respectively, per sample, which are much better than those attainable by AS [50 fg (∼115.3 µBq) of (239)Pu per sample, approximately]. Therefore, it is demonstrated that the MS techniques employed in this work are very powerful tools for internal dosimetry studies in human urine samples, giving excellent results when the reassessment of AS planchets is needed (samples with a Pu concentration below or at the MDA levels measurable by AS). This work is the continuation of an article published in J. Anal. At. Spectrom. 25 (1410-1415) 2010.

  5. Fabrication of aluminum terephthalate metal-organic framework incorporated polymer monolith for the microextraction of non-steroidal anti-inflammatory drugs in water and urine samples.

    Science.gov (United States)

    Lyu, Dan-Ya; Yang, Cheng-Xiong; Yan, Xiu-Ping

    2015-05-08

    Polymer monolith microextraction (PMME) based on capillary monolithic column is an effective and useful technique to preconcentrate trace analytes from environmental and biological samples. Here, we report the fabrication of a novel aluminum terephthalate metal-organic framework (MIL-53(Al)) incorporated capillary monolithic column via in situ polymerization for the PMME of non-steroidal anti-inflammatory drugs (NSAIDs) (ketoprofen, fenbufen and ibuprofen) in water and urine samples. The fabricated MIL-53(Al) incorporated monolith was characterized by X-ray powder diffractometry, scanning electron microscopy, Fourier transform infrared spectrometry, and nitrogen adsorption experiment. The MIL-53(Al) incorporated monolith gave larger surface area than the neat polymer monolith. A 2-cm long MIL-53(Al) incorporated capillary monolith was applied for PMME coupled with high-performance liquid chromatography for the determination of the NSAIDs. Potential factors affecting the PMME were studied in detail. Under the optimized conditions, the developed method gave the enhancement factors of 46-51, the linear range of 0.40-200μgL(-1), the detection limits (S/N=3) of 0.12-0.24μgL(-1), and the quantification limits (S/N=10) of 0.40-0.85μgL(-1). The recoveries for spiked NSAIDs (20μgL(-1)) in water and urine samples were in the range of 77.3-104%. Besides, the MIL-53(Al) incorporated monolith was stable enough for 120 extraction cycles without significant loss of extraction efficiency. The developed method was successfully applied to the determination of NSAIDs in water and urine samples.

  6. A competitive immunoassay for ultrasensitive detection of Hg(2+) in water, human serum and urine samples using immunochromatographic test based on surface-enhanced Raman scattering.

    Science.gov (United States)

    She, Pei; Chu, Yanxin; Liu, Chunwei; Guo, Xun; Zhao, Kang; Li, Jianguo; Du, Haijing; Zhang, Xiang; Wang, Hong; Deng, Anping

    2016-02-01

    An immunochromatographic test (ICT) strip was developed for ultrasensitive competitive immunoassay of Hg(2+). This strategy was achieved by combining the easy-operation and rapidity of ICT with the high sensitivity of surface-enhanced Raman scattering (SERS). Monoclonal antibody (mAb) against Hg(2+) and Raman active substance 4-mercaptobenzoic acid (MBA) dual labelled gold nanoparticles (GNPs) were prepared as an immunoprobe. The Raman scattering intensity of MBA on the test line of the ICT strip was measured for quantitative determination of Hg(2+). The ICT was able to directly detect Hg(2+) without complexing due to the specific recognition of the mAb with Hg(2+). The IC50 and limit of detection (LOD) of the assay for Hg(2+) detection were 0.12 ng mL(-1) and 0.45 pg mL(-1), respectively. There was no cross-reactivity (CR) of the assay with other nineteen ions and the ICT strips could be kept for 5 weeks without loss of activity. The recoveries of the assay for water, human serum and urine samples spiked with Hg(2+) were in range of 88.3-107.3% with the relative standard deviations (RSD) of 1.5-9.5% (n = 3). The proposed ICT was used for the detection of Hg(2+) in urine samples collected from Occupational Disease Hospital and the results were confirmed by cold-vapor atomic fluorescence spectroscopy (CV-AFS). The assay exhibited high sensitivity, selectivity, stability, precision and accuracy, demonstrating a promising method for the detection of trace amount of Hg(2+) in environmental water samples and biological serum and urine samples.

  7. Combination with antimicrobial peptide lyses improves loop-mediated isothermal amplification based method for Chlamydia trachomatis detection directly in urine sample.

    Science.gov (United States)

    Jevtuševskaja, Jekaterina; Uusna, Julia; Andresen, Liis; Krõlov, Katrin; Laanpere, Made; Grellier, Tiia; Tulp, Indrek; Langel, Ülo

    2016-07-13

    Chlamydia trachomatis is an obligate intracellular human pathogen and is the most common cause of sexually transmitted diseases affecting both men and women. The pathogen can cause prostatitis and epididymitis in men. In women, cervicitis, pelvic inflammatory disease, ectopic pregnancy and acute or chronic pelvic pain are frequent complications. More than half of C. trachomatis-positive patients have minimal or no symptoms, providing an ongoing reservoir for the infection. The lack of sensitive large-scale applicable point- of- care (POC) tests for C. trachomatis detection makes it difficult to diagnose chlamydia infection efficiently in resource-limited environments. A rapid and sensitive assay based on loop-mediated isothermal amplification method (LAMP) was combined with antimicrobial peptide lysis, which is able to detect at least 7 C. trachomatis pathogens per reaction directly from urine samples. Our study comprising 91 first-void urine samples showed that specificity of the assay is 100 % and sensitivity 73 % when using antimicrobial peptide lysis mix. Additionally we demonstrate that our assay does not give any cross-reactivity with 30 pathogen's DNA potentially present in the urine samples. Furthermore, the assay's novel approach does not require purification or extraction of DNA from clinical sample prior to amplification, so the need for specialized equipment is eliminated. The whole procedure is significantly less laborious, less time-consuming and consequently less expensive for early detection and identification of infectious disease. C. trachomatis specific LAMP assay is relatively simple to perform and could therefore be applied in numerous POC settings.

  8. On the performance of multiway methods for simultaneous quantification of two fluoroquinolones in urine samples by fluorescence spectroscopy and second-order calibration strategies

    Science.gov (United States)

    Vosough, Maryam; Eshlaghi, Sara Noroozi; Zadmard, Reza

    2015-02-01

    In the present work, the analytical performance of three multi-way algorithms has been evaluated. The proposed analytical problem was the simultaneous determination of moxifloxacin and ciprofloxacin in human urine samples using fluorescence spectroscopy. Parallel factor analysis (PARAFAC), self-weighted alternating trilinear decomposition (SWATLD) and unfolded partial least squares combined with the residual bilinearization procedure (U-PLS/RBL) have been compared, regarding their ability to solve the proposed problem. In this study, "second-order advantage" was also exploited for the mentioned algorithms through different calibration strategies. The three-way data was obtained via fluorescence spectroscopy, so that excitation-emission matrices (EEM) of the samples were recorded as the analytical signals. The accuracy and precision of each individual algorithm for analyzing the drugs in urine samples were compared using root mean square error of prediction (RMSEP), recovery and elliptical joint confidence region (EJCR) plots. The results revealed that each of the three algorithms could be applied for determination of moxifloxacin and ciprofloxacin, despite different EEM subsets and calibration strategies. However, better analytical performances were observed through PARAFAC and U-PLS/RBL modeling for MOX and CIP, respectively. So, by coupling the multi-way decomposition algorithms with fluorescence spectroscopy, a main part of preliminary sample preparation steps can be eliminated and experimental procedure might be significantly simplified, while achieving desirable analytical performance.

  9. Determination of parabens in urine samples by microextraction using packed sorbent and ultra-performance liquid chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Cristina Jardim, Valeria; de Paula Melo, Lidervan; Soares Domingues, Diego; Costa Queiroz, Maria Eugênia

    2015-01-01

    A simple, sensitive, and selective method using ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) was developed and validated for simultaneous determination of parabens [methyl paraben (MeP), ethyl paraben (EtP), propyl paraben (PrP), butyl paraben (BuP), and benzyl paraben (BzP)] in human urine samples. After microextraction by packed sorbent (MEPS) using a C18 phase, the parabens were separated on a Kinetex C18 column (100 mm × 2.1 mm × 1.7 μm) within 4.6 min using isocratic elution. These compounds were detected on a triple quadrupole tandem mass spectrometer using the multiple reactions monitoring (MRM) mode via an electrospray ionization source operating in the negative ionization mode. Important factors that influence MEPS performance were evaluated, such as the sample pH, draw-eject sample volume, clean-up step, and desorption conditions. The proposed MEPS/UPLC-MS/MS method presented a linear range from 0.5 ng mL(-1) (limit of quantification - LOQ) to 50 ng mL(-1), and interassay precision with coefficients of variation lower than 15%, and relative standard error values of the accuracy ranged from -8.8% to 15%. The MEPS/UPLC-MS/MS method was applied successfully to determine parabens in urine samples from 30 postpartum volunteers, enabling assessment of human exposure to these compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Solidified floating organic drop microextraction combined with high performance liquid chromatography for the determination of carbamazepine in human plasma and urine samples

    Institute of Scientific and Technical Information of China (English)

    Mohammad ASADI; Ali Mohammad HAJI SHABANI; Shayessteh DADFARNIA; Bijan ABBASI

    2015-01-01

    Solidified floating organic drop microextraction( SFODME)in combination with high performance liquid chromatography was used for separation/preconcentration and determination of carbamazepine( CBZ)in human plasma and urine samples. Parameters that affect the extraction efficiency such as the type and volume of extraction solvent,ionic strength,sodium hydroxide concentration,stirring rate,sample volume and extrac-tion time,were investigated and optimized. Under the optimum conditions( extraction solvent,40 μL of 1-un-decanol;sodium hydroxide concentration,1 mol/L;temperature,50 ℃;stirring speed,400 r/min;sample vol-ume,8 mL;sodium chloride concentration,3%( w/v)and extraction time,60 min)the calibration curve was found to be linear in the mass concentration range of 0. 4-700. 0 μg/L. The limit of detection( LOD)was 0. 1μg/L and the relative standard deviation( RSD)for six replicate extraction and determination of carbamazepine at 100 μg/L level was found to be 4. 1%. The method was successfully applied to the determination of CBZ in human plasma and urine samples.

  11. UHPLC-MS/MS method for the determination of bisphenol A and its chlorinated derivatives, bisphenol S, parabens, and benzophenones in human urine samples.

    Science.gov (United States)

    Vela-Soria, F; Ballesteros, O; Zafra-Gómez, A; Ballesteros, L; Navalón, A

    2014-06-01

    In the present work, a new method based on a sample treatment by dispersive liquid-liquid microextraction (DLLME) for the extraction of six bisphenols (bisphenol A, bisphenol S, and monochloro-, dichloro-, trichloro-, and tetrachlorobisphenol A), four parabens (methyl-, ethyl-, propyl-, and butylparaben), and six benzophenones (benzophenone-1, benzophenone-2, benzophenone-3, benzophenone-6, benzophenone-8, and 4-hydroxybenzophenone) in human urine samples, followed by ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis, is validated. An enzymatic treatment allows determining the total content of the target EDCs. The extraction parameters were accurately optimized using multivariate optimization strategies. Ethylparaben ring-(13)C6, benzophenone-d10, and bisphenol A-d16 were used as surrogates. Limits of quantification ranging from 0.1 to 0.6 ng mL(-1) and interday variabilities (evaluated as relative standard deviations) from 2.0 to 13.8% were obtained. The method was validated using matrix-matched standard calibration followed by a recovery assay with spiked samples. Recovery rates ranged from 94 to 106%. A good linearity, for concentrations up to 300 ng mL(-1) for parabens and 40 ng mL(-1) for benzophenones and bisphenols, was also obtained. The method was satisfactorily applied for the determination of target compounds in human urine samples from 20 randomly selected individuals.

  12. Electrochemical detection of toxic ractopamine and salbutamol in pig meat and human urine samples by using poly taurine/zirconia nanoparticles modified electrodes.

    Science.gov (United States)

    Rajkumar, Muniyandi; Li, Ying-Sheng; Chen, Shen-Ming

    2013-10-01

    Detection of ractopamine and salbutamol has been developed by employing the facile synthesis of poly taurine/zirconia nanoparticles (ZrO2) modified film glassy carbon electrode. The poly taurine/ZrO2 nanoparticles were directly utilized for the detection of ractopamine and salbutamol using linear sweep voltammetry (LSV). The modified electrode successfully shows the oxidation peak for ractopamine adsorption at 0.65V and salbutamol at 0.71V, which is purely based on the detection of adsorption signals of ractopamine and salbutamol, at the electrode surface. Furthermore, the electrochemical measurements and surface morphology were studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) analysis. The modified electrode successfully detects the oxidation signals of ractopamine in the linear range of 1-28μM and salbutamol in the linear range of 5-220μM in laboratory samples. The proposed film also successfully detects the ractopamine signal (1-26μM) in pig meat samples and salbutamol signal (1-114μM) in human urine samples. It also exhibits two well-separated anodic oxidation peaks for uric acid and salbutamol in salbutamol-spiked human urine samples.

  13. Utility of slot-blot-ELISA as a new, fast, and sensitive immunoassay for detection of carcinoembryonic antigen in the urine samples of patients with various gastrointestinal malignancies.

    Science.gov (United States)

    El-Masry, Samir; El-Sayed, Ibrahim H; Lotfy, Mahmoud; Mahmoud, Lamiaa; El-Naggar, Mohamed

    2007-01-01

    Carcinoembryonic antigen (CEA) is the most widely used clinical tumor marker. CEA immunoassay has found acceptance as a diagnostic adjunct in clinical diagnosis of gastrointestinal tumors (GIT). Several immunoassays have been established for detection of CEA in plasma, serum, tissue, feces, and urine of cancer patients using polyclonal or monoclonal antibodies raised against CEA. Some of these assays display both high sensitivity and specificity for the detection of CEA. However, these assays require special and highly expensive equipment and the procedures require long periods for their completion. In the present study, we established a Slot-Blot Enzyme Linked Immunosorbent Assay (SB-ELISA), based on anti-CEA monoclonal antibody (CEA-mAb), as a new, simple, fast, cheap, and non-invasive immunodiagnostic technique for detection of CEA in the urine of GIT patients. Urine and serum samples were collected from 248 GIT patients (58 with pancreatic cancer, 20 with hepatoma, 23 with ampullary carcinoma, 15 with hilar cholangiocarcinoma, 28 with gastric cancer, 14 with esophageal cancer, and 90 with colorectal cancer). Moreover, urine and serum samples were collected from 50 healthy individuals to serve as negative controls. The traditional ELISA technique was used for determination of CEA in the sera of GIT patients using anti-CEA monoclonal antibody. A comparison between the results of both techniques (ELISA and SB-ELISA) was carried out. The traditional ELISA detected CEA in the sera of 154 out of 248 GIT patients with a sensitivity of 59.8%, 51.7% positive predictive value (PPV) and 75.37% negative predictive value (NPV). In addition, it identified 15 false positive cases out of 50 healthy individuals with a specificity of 70%. The urinary CEA was identified by a Western blotting technique and CEA-mAb at a molecular mass of 180 Kda. The developed SB-ELISA showed higher sensitivity, specificity, PPV, and NPV (70.1%, 78%, 62.4%, and 82.13%, respectively) for detection

  14. Hydrophilic interaction chromatography combined with dispersive liquid-liquid microextraction as a preconcentration tool for the simultaneous determination of the panel of underivatized neurotransmitters in human urine samples.

    Science.gov (United States)

    Konieczna, Lucyna; Roszkowska, Anna; Niedźwiecki, Maciej; Bączek, Tomasz

    2016-01-29

    A simple and sensitive method using dispersive liquid-liquid microextraction (DLLME) followed by liquid chromatography coupled to mass spectrometry (LC-MS) with a hydrophilic interaction chromatography (HILIC) column was developed for the simultaneous determination of 13 compounds of different polarities, comprising monoamine neurotransmitters (dopamine, norepinephrine, epinephrine and serotonin) along with their respective precursors and metabolites, in human urine samples. The microextraction procedure was based on the fast injection of a mixture of ethanol (disperser solvent) and dichloromethane (extraction solvent) into a human urine sample, forming a cloudy solution in the Eppendorf tube. After centrifugation, the sedimented phase was collected and subsequently analyzed by LC-HILIC-MS in about 12min without a derivatization step. The separation was performed on an XBridge Amide™ BEH column 3.0×100mm, 3.5mm and the mobile phase consisted of phase A: 10mM ammonium formate buffer in water pH 3.0 and phase B: 10 mM ammonium formate buffer in acetonitrile, under gradient program elution. Tyrosine, tryptophan, 5-hydroxytryptophan, dopamine, epinephrine, norepinephrine, serotonin, 3-methoxytyramine, 5-hydroxyindole-3-acetic acid, 3,4-dihydroxy-l-phenylalanine and norvaline (internal standard) were detected in the positive ionization mode. While vanillylmandelic acid, homovanillic acid, 3,4-dihydroxyphenylacetic acid and 3,4-dihydroxybenzylamine (internal standard) were detected in the negative ionization mode. Parameters influencing DLLME and LC-HILIC-MS were investigated. Under the optimum conditions, the proposed method exhibited a low detection limit (5-10ngmL(-1)), and good linearity with R between 0.9991 and 0.9998. The recoveries in human urine samples were 99.0%±3.6%. for the 13 studied biogenic amines with intra- and inter-day RSDs of 0.24-9.55% and 0.31-10.0%, respectively. The developed DLLME-LC-MS method could be successfully applied for the

  15. A competitive immunoassay for ultrasensitive detection of Hg{sup 2+} in water, human serum and urine samples using immunochromatographic test based on surface-enhanced Raman scattering

    Energy Technology Data Exchange (ETDEWEB)

    She, Pei; Chu, Yanxin [The Key Lab of Health Chemistry & Molecular Diagnosis of Suzhou, College of Chemistry, Chemical Engineering & Materials Science, Soochow University, Renai Road 199, Suzhou 215123 (China); Liu, Chunwei; Guo, Xun [OptoTrace (Suzhou) Technologies, Inc., STE 316, Building 4, No. 218, Xinghu Street, bioBAY, Suzhou Industrial Park, Suzhou 215123 (China); Zhao, Kang [The Key Lab of Health Chemistry & Molecular Diagnosis of Suzhou, College of Chemistry, Chemical Engineering & Materials Science, Soochow University, Renai Road 199, Suzhou 215123 (China); Li, Jianguo, E-mail: lijgsd@suda.edu.cn [The Key Lab of Health Chemistry & Molecular Diagnosis of Suzhou, College of Chemistry, Chemical Engineering & Materials Science, Soochow University, Renai Road 199, Suzhou 215123 (China); Du, Haijing; Zhang, Xiang [The Key Lab of Health Chemistry & Molecular Diagnosis of Suzhou, College of Chemistry, Chemical Engineering & Materials Science, Soochow University, Renai Road 199, Suzhou 215123 (China); Wang, Hong [OptoTrace (Suzhou) Technologies, Inc., STE 316, Building 4, No. 218, Xinghu Street, bioBAY, Suzhou Industrial Park, Suzhou 215123 (China); Deng, Anping, E-mail: denganping@suda.edu.cn [The Key Lab of Health Chemistry & Molecular Diagnosis of Suzhou, College of Chemistry, Chemical Engineering & Materials Science, Soochow University, Renai Road 199, Suzhou 215123 (China)

    2016-02-04

    An immunochromatographic test (ICT) strip was developed for ultrasensitive competitive immunoassay of Hg{sup 2+}. This strategy was achieved by combining the easy-operation and rapidity of ICT with the high sensitivity of surface-enhanced Raman scattering (SERS). Monoclonal antibody (mAb) against Hg{sup 2+} and Raman active substance 4-mercaptobenzoic acid (MBA) dual labelled gold nanoparticles (GNPs) were prepared as an immunoprobe. The Raman scattering intensity of MBA on the test line of the ICT strip was measured for quantitative determination of Hg{sup 2+}. The ICT was able to directly detect Hg{sup 2+} without complexing due to the specific recognition of the mAb with Hg{sup 2+}. The IC{sub 50} and limit of detection (LOD) of the assay for Hg{sup 2+} detection were 0.12 ng mL{sup −1} and 0.45 pg mL{sup −1}, respectively. There was no cross-reactivity (CR) of the assay with other nineteen ions and the ICT strips could be kept for 5 weeks without loss of activity. The recoveries of the assay for water, human serum and urine samples spiked with Hg{sup 2+} were in range of 88.3–107.3% with the relative standard deviations (RSD) of 1.5–9.5% (n = 3). The proposed ICT was used for the detection of Hg{sup 2+} in urine samples collected from Occupational Disease Hospital and the results were confirmed by cold-vapor atomic fluorescence spectroscopy (CV-AFS). The assay exhibited high sensitivity, selectivity, stability, precision and accuracy, demonstrating a promising method for the detection of trace amount of Hg{sup 2+} in environmental water samples and biological serum and urine samples. - Highlights: • The proposed ICT was able to directly detect Hg{sup 2+} without formation of Hg{sup 2+}-ligand complex. • The proposed ICT exhibited high sensitivity, specificity, stability, precision and accuracy for Hg{sup 2+} detection. • The proposed ICT was applicable for the detection of trace amount of Hg{sup 2+} in water, human serum and urine samples.

  16. Organophosphate Insecticide Metabolites in Prenatal and Childhood Urine Samples and Intelligence Scores at 6 Years of Age: Results from the Mother–Child PELAGIE Cohort (France)

    Science.gov (United States)

    Cartier, Chloé; Warembourg, Charline; Le Maner-Idrissi, Gaïd; Lacroix, Agnès; Rouget, Florence; Monfort, Christine; Limon, Gwendolina; Durand, Gaël; Saint-Amour, Dave; Cordier, Sylvaine; Chevrier, Cécile

    2015-01-01

    Background: Several studies suggest that exposure to organophosphate insecticides (OP) during pregnancy impairs neurodevelopment in children. Objectives: We evaluated associations between biomarkers of prenatal and postnatal OP exposure and cognitive function of 6-year-olds in a French longitudinal birth cohort. Methods: In 2002–2006, the PELAGIE mother–child cohort enrolled pregnant women from Brittany. For a random subcohort, we measured nonspecific dialkylphosphate metabolites (DAP) of OP in one maternal urine sample, collected before 19 weeks’ gestation, and in one urine sample collected from their 6-year-old children. Six subtests of the Wechsler Intelligence Scale for Children, 4th edition (WISC-IV) were administered when the children were 6 years of age to evaluate cognitive function (n = 231). Linear regression models controlling for factors including maternal intelligence and the Home Observation for Measurement of the Environment score were used. Results: WISC-IV scores were not significantly associated with prenatal or childhood total DAP metabolites. WISC verbal comprehension score was significantly higher in association with the highest maternal urinary concentrations of diethylphosphate (DE) metabolites (5.5; 95% CI: 0.8, 10.3 for > 13.2 nmol/L vs. WISC working memory score was significantly lower in association with the highest urinary concentrations of DE metabolites at age 6 years (–3.6; 95% CI: –7.8, –0.6 for > 11.1 nmol/L vs. WISC score and concurrent DE urinary concentrations requires replication by longitudinal studies investigating childhood OP exposure. Citation: Cartier C, Warembourg C, Le Maner-Idrissi G, Lacroix A, Rouget F, Monfort C, Limon G, Durand G, Saint-Amour D, Cordier S, Chevrier C. 2016. Organophosphate insecticide metabolites in prenatal and childhood urine samples and intelligence scores at 6 years of age: results from the mother–child PELAGIE cohort (France). Environ Health Perspect 124:674–680; http

  17. Organophosphate Insecticide Metabolites in Prenatal and Childhood Urine Samples and Intelligence Scores at 6 Years of Age: Results from the Mother-Child PELAGIE Cohort (France).

    Science.gov (United States)

    Cartier, Chloé; Warembourg, Charline; Le Maner-Idrissi, Gaïd; Lacroix, Agnès; Rouget, Florence; Monfort, Christine; Limon, Gwendolina; Durand, Gaël; Saint-Amour, Dave; Cordier, Sylvaine; Chevrier, Cécile

    2016-05-01

    Several studies suggest that exposure to organophosphate insecticides (OP) during pregnancy impairs neurodevelopment in children. We evaluated associations between biomarkers of prenatal and postnatal OP exposure and cognitive function of 6-year-olds in a French longitudinal birth cohort. In 2002-2006, the PELAGIE mother-child cohort enrolled pregnant women from Brittany. For a random subcohort, we measured nonspecific dialkylphosphate metabolites (DAP) of OP in one maternal urine sample, collected before 19 weeks' gestation, and in one urine sample collected from their 6-year-old children. Six subtests of the Wechsler Intelligence Scale for Children, 4th edition (WISC-IV) were administered when the children were 6 years of age to evaluate cognitive function (n = 231). Linear regression models controlling for factors including maternal intelligence and the Home Observation for Measurement of the Environment score were used. WISC-IV scores were not significantly associated with prenatal or childhood total DAP metabolites. WISC verbal comprehension score was significantly higher in association with the highest maternal urinary concentrations of diethylphosphate (DE) metabolites (5.5; 95% CI: 0.8, 10.3 for > 13.2 nmol/L vs. WISC working memory score was significantly lower in association with the highest urinary concentrations of DE metabolites at age 6 years (-3.6; 95% CI: -7.8, -0.6 for > 11.1 nmol/L vs. WISC score and concurrent DE urinary concentrations requires replication by longitudinal studies investigating childhood OP exposure. Cartier C, Warembourg C, Le Maner-Idrissi G, Lacroix A, Rouget F, Monfort C, Limon G, Durand G, Saint-Amour D, Cordier S, Chevrier C. 2016. Organophosphate insecticide metabolites in prenatal and childhood urine samples and intelligence scores at 6 years of age: results from the mother-child PELAGIE cohort (France). Environ Health Perspect 124:674-680; http://dx.doi.org/10.1289/ehp.1409472.

  18. Urine Odor

    Science.gov (United States)

    ... References Brunzel NA. Physical examination of urine. In: Fundamentals of Urine and Body Fluid Analysis. 3rd ed. St. Louis, Mo.: Saunders Elsevier; 2013:97. McPherson RA, et al., eds. Henry's Clinical Diagnosis and Management by Laboratory Methods. 23rd ed. St. Louis, Mo.: ...

  19. On the sequential separation and quantification of (237)Np, (241)Am, thorium, plutonium, and uranium isotopes in environmental and urine samples.

    Science.gov (United States)

    Vasile, M; Jacobs, K; Bruggeman, M; Van Hoecke, K; Dobney, A; Verrezen, F

    2017-07-13

    The implementation of the one-pass-through separation technique using two stacked chromatography columns of TEVA - TRU resins for the separation of (237)Np, (241)Am, thorium, plutonium and uranium from environmental and urine samples was investigated. The sequential separation technique proved to be successful and gave similar results to those obtained when using individual separations. The analysis time was considerably improved. The amount of chemical waste was also reduced by 50% and the use of HClO4 was avoided. The technique of ICP-MS was also investigated as a complementary technique to alpha-spectrometry. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Visual and colorimetric detection of p-aminophenol in environmental water and human urine samples based on anisotropic growth of Ag nanoshells on Au nanorods.

    Science.gov (United States)

    Lin, Tianran; Li, Zhihong; Song, Zhiping; Chen, Huan; Guo, Liangqia; Fu, Fengfu; Wu, Zujian

    2016-01-01

    A simple, sensitive, selective and high-resolution colorimetric method has been developed for the detection of p-aminophenol in environmental water and human urine samples. In the presence of p-aminophenol, silver ions are reduced to silver atoms and subsequently Ag nanoshells anisotropically grow on the surface of Au nanorods to generate orange slice-like Au@Ag core-shell nanocrystals, thereby resulting in the blue-shift of longitudinal surface plasmon resonance band of Au nanorods accompanying a sharp-contrast multicolor change. Using Au@Ag core-shell nanocrystals as the transducer, sub-micromolar p-aminophenol can be detected by the colorimetric method and 10 μmol L(-1) p-aminophenol can be visual readout by the naked eyes. Furthermore, a simple, cheap, portable test kit is constructed for the visual assay of urinary p-aminophenol without complicated sample pretreatment and sophisticated instruments. The proposed colorimetric method has the potential for the rapid and on-site analyses of p-aminophenol in environmental water and human urine samples.

  1. Liquid chromatography-quadrupole-time-of-flight mass spectrometry screening procedure for urine samples in forensic casework compared to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fels, Helena; Dame, Torsten; Sachs, Hans; Musshoff, Frank

    2016-07-04

    This work represents the development, validation, and application of a liquid chromatography-quadrupole-time-of-flight mass spectrometry (LC-QTOF-MS) screening method for the detection of pharmaceutical substances and illicit drugs (acidic, basic, and neutral organic drugs) in urine samples. Time-of-flight mass spectrometry was performed using an LC-Triple TOF 5600 system with electrospray ionization operated in both positive and negative mode, respectively. The limits of detection (LODs), determined for 34 substances, were 70%). These four parameters served as identification criteria and are discussed according to their role in identifying compounds even without reference substances. In routine casework, two in-house XIC (extracted ion chromatogram) lists, consisting of 456 protonated and 26 deprotonated compounds were used and retention times for 365 compounds were available. Compared to the results found with the established gas chromatography-mass spectrometry (GC-MS) procedure, the findings with the LC-QTOF-MS screening method showed a good comparability. Results that were not detected by LC-QTOF-MS because of a missing entry in the targeted XIC list could retrospectively be confirmed by simply entering the elemental formula of the relevant substance into the software and reprocessing the sample. LC-QTOF-MS offers an attractive technique for the fast and specific identification of illicit drugs and toxic compounds in urine samples. Copyright © 2016 John Wiley & Sons, Ltd.

  2. Gas chromatography – mass spectrometry of JWH-018 metabolites in urine samples with direct comparison to analytical standards

    Science.gov (United States)

    Emerson, Beth; Durham, Bill; Gidden, Jennifer; Lay, Jackson O.

    2013-01-01

    JWH-018 (1-pentyl-3-(1-naphthoyl)indole) is one of numerous potential aminoalkylindoles contained in products marketed as ‘K2’ or ‘Spice’. Investigation of the urinary metabolites from consumption of these compounds is important because they are banned in the United States and many European countries. An efficient extraction procedure and gas chromatography – mass spectrometry (GC-MS) method were developed for detection of ‘K2’ metabolites in urine from individuals suspected of using these products. Analytical standards were used to elucidate the structure-specific mass spectral fragmentations and retention properties to confirm proposed identifications and support quantitative studies. A procedure for the synthesis of one of these metabolites (5-hydroxypentyl JWH-018) was also developed. Results are comparable to existing LC-MS/MS methods, with the same primary metabolites detected. The specific metabolite hydrolysis products include 4-hydroxpentyl, 5-hydroxypentyl, and N-pentanoic acid derivatives. PMID:23683902

  3. Generation of integration free induced pluripotent stem cells from fibrodysplasia ossificans progressiva (FOP) patients from urine samples.

    Science.gov (United States)

    Hildebrand, Laura; Rossbach, Bella; Kühnen, Peter; Gossen, Manfred; Kurtz, Andreas; Reinke, Petra; Seemann, Petra; Stachelscheid, Harald

    2016-01-01

    Fibrodysplasia ossificans progressiva (FOP) is an extremely rare, autosomal dominant transmitted genetic disease. Patients experience progressive bone formation replacing tendons, ligaments, muscle and soft tissue. Cause of FOP are gain-of-function mutations in the Bone Morphogenetic Protein (BMP) receptor Activin A receptor type 1 (ACVR1) (Kaplan et al., 2008). The most common mutation is R206H, which leads to the substitution of codon 206 from arginine to histidine (Shore et al., 2006). Here, we describe the derivation and characterization of two hiPSC lines from two FOP patients, both carrying the mutation R206H. Cells were isolated from urine and reprogrammed using integration free Sendai virus vectors under defined conditions.

  4. Metabolomic profiling of urine samples from mice exposed to protons reveals radiation quality and dose specific differences.

    Science.gov (United States)

    Laiakis, Evagelia C; Trani, Daniela; Moon, Bo-Hyun; Strawn, Steven J; Fornace, Albert J

    2015-04-01

    As space travel is expanding to include private tourism and travel beyond low-Earth orbit, so is the risk of exposure to space radiation. Galactic cosmic rays and solar particle events have the potential to expose space travelers to significant doses of radiation that can lead to increased cancer risk and other adverse health consequences. Metabolomics has the potential to assess an individual's risk by exploring the metabolic perturbations in a biofluid or tissue. In this study, C57BL/6 mice were exposed to 0.5 and 2 Gy of 1 GeV/nucleon of protons and the levels of metabolites were evaluated in urine at 4 h after radiation exposure through liquid chromatography coupled to time-of-flight mass spectrometry. Significant differences were identified in metabolites that map to the tricarboxylic acid (TCA) cycle and fatty acid metabolism, suggesting that energy metabolism is severely impacted after exposure to protons. Additionally, various pathways of amino acid metabolism (tryptophan, tyrosine, arginine and proline and phenylalanine) were affected with potential implications for DNA damage repair and cognitive impairment. Finally, presence of products of purine and pyrimidine metabolism points to direct DNA damage or increased apoptosis. Comparison of these metabolomic data to previously published data from our laboratory with gamma radiation strongly suggests a more pronounced effect on metabolism with protons. This is the first metabolomics study with space radiation in an easily accessible biofluid such as urine that further investigates and exemplifies the biological differences at early time points after exposure to different radiation qualities.

  5. Novel DFO-functionalized mesoporous silica for iron sensing. Part 2. Experimental detection of free iron concentration (pFe) in urine samples.

    Science.gov (United States)

    Alberti, Giancarla; Emma, Giovanni; Colleoni, Roberta; Pesavento, Maria; Nurchi, Valeria Marina; Biesuz, Raffaela

    2014-08-21

    Successful in vivo chelation treatment of iron(iii) overload pathologies requires that a significant fraction of the administered drug actually chelates the toxic metal. Increased mobilization of the iron(iii) in experiments on animals or humans, most often evaluated from urinary output, is usually used as an assessment tool for chelation therapy. Alternatively, the efficiency of a drug is estimated by calculating the complexing ability of a chelating agent towards Fe(iii). The latter is calculated by the pFe value, defined as the negative logarithm of the concentration of the free metal ion in a solution containing 10 μM total ligand and 1 μM total metal at a physiological pH of 7.4. In theory, pFe has to be calculated taking into account all the complexation equilibria involving the metal and the possible ligands. Nevertheless, complexation reactions in complex systems such as serum and urine may hardly be accurately modelled by computer software. The experimental determination of the bioavailable fraction of iron(iii) in biological fluids would therefore be of the utmost relevance in the clinical practice. The efficiency of the therapy could be more easily estimated as well as the course of overload pathologies. In this context, the aim of the present work was the development of a sensor to assess the free iron directly in biological fluids (urine) of patients under treatment with chelating agents. In the proposed device (DFO-MS), the strong iron chelator deferoxamine (DFO) is immobilized on the MCM-41 mesoporous silica. The characterization of the iron(iii) sorption on DFO-MS was undertaken, firstly in 0.1 M KNO3, then directly in urine samples, in order to identify the sorption mechanism. The stoichiometry of the reaction in the solid phase was found to be: with an exchange constant (average value) of log βex = 40(1). The application of DFO-MS to assess pFe in SPU (Simulating Pathology Urine) samples was also considered. The results obtained were very

  6. Molecularly imprinted polymer microspheres prepared by Pickering emulsion polymerization for selective solid-phase extraction of eight bisphenols from human urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jiajia [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Li, Yun; Wang, Jincheng [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Sun, Xiaoli; Cao, Rong [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Sun, Hao [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); Department of Chemistry, Liaoning University, Shenyang 110000 (China); Huang, Chaonan [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China); University of Chinese Academy of Sciences, Beijing 100049 (China); Chen, Jiping, E-mail: chenjp@dicp.ac.cn [Key Laboratory of Separation Sciences for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023 (China)

    2015-05-04

    Highlights: • BPA imprinted polymer microspheres were prepared by Pickering emulsion polymerization. • Regular spherical shape and narrow diameter distribution. • Good specific adsorption capacity for BPA. • Good class-selectivity and clean-up efficiency for bisphenols in human urine under SPE mode. • Good recoveries and sensitivity for bisphenols using the MIPMS-SPE coupled with HPLC-DAD method. - Abstract: The bisphenol A (BPA) imprinted polymer microspheres were prepared by simple Pickering emulsion polymerization. Compared to traditional bulk polymerization, both high yields of polymer and good control of particle sizes were achieved. The characterization results of scanning electron microscopy and nitrogen adsorption–desorption measurements showed that the obtained molecularly imprinted polymer microsphere (MIPMS) particles possessed regular spherical shape, narrow diameter distribution (30–60 μm), a specific surface area (S{sub BET}) of 281.26 m{sup 2} g{sup −1} and a total pore volume (V{sub t}) of 0.459 cm{sup 3} g{sup −1}. Good specific adsorption capacity for BPA was obtained in the sorption experiment and good class selectivity for BPA and its seven structural analogs (bisphenol F, bisphenol B, bisphenol E, bisphenol AF, bisphenol S, bisphenol AP and bisphenol Z) was demonstrated by the chromatographic evaluation experiment. The MIPMS as solid-phase extraction (SPE) packing material was then evaluated for extraction and clean-up of these bisphenols (BPs) from human urine samples. An accurate and sensitive analytical method based on the MIPMS-SPE coupled with HPLC-DAD has been successfully established for simultaneous determination of eight BPs from human urine samples with detection limits of 1.2–2.2 ng mL{sup −1}. The recoveries of BPs for urine samples at two spiking levels (100 and 500 ng mL{sup −1} for each BP) were in the range of 81.3–106.7% with RSD values below 8.3%.

  7. Validation of the method for determination of plutonium isotopes in urine samples and its application in a nuclear facility at Otwock

    Directory of Open Access Journals (Sweden)

    Rzemek Katarzyna

    2015-03-01

    Full Text Available The studies aimed at determining low activities of alpha radioactive elements are widely recognized as essential for the human health, because of their high radiotoxicity in case of internal contamination. Some groups of workers of nuclear facility at Otwock are potentially exposed to contamination with plutonium isotopes. For this reason, the method for determination of plutonium isotopes has been introduced and validated in Radiation Protection Measurements Laboratory (LPD of the National Centre for Nuclear Research (NCBJ. In this method the plutonium is isolated from a sample by coprecipitation with phosphates and separated on a AG 1-X2 Resin. After electrodeposition, the sample is measured by alpha spectrometry. Validation was performed in order to assess parameters such as: selectivity, accuracy (trueness and precision and linearity of the method. The results of plutonium determination in urine samples of persons potentially exposed to internal contamination are presented in this work.

  8. Evaluating 3D printing to solve the sample-to-device interface for LRS and POC diagnostics: example of an interlock meter-mix device for metering and lysing clinical urine samples.

    Science.gov (United States)

    Jue, Erik; Schoepp, Nathan G; Witters, Daan; Ismagilov, Rustem F

    2016-05-21

    This paper evaluates the potential of 3D printing, a semi-automated additive prototyping technology, as a means to design and prototype a sample-to-device interface, amenable to diagnostics in limited-resource settings, where speed, accuracy and user-friendly design are critical components. As a test case, we built and validated an interlock meter-mix device for accurately metering and lysing human urine samples for use in downstream nucleic acid amplification. Two plungers and a multivalve generated and controlled fluid flow through the device and demonstrate the utility of 3D printing to create leak-free seals. Device operation consists of three simple steps that must be performed sequentially, eliminating manual pipetting and vortexing to provide rapid (5 to 10 s) and accurate metering and mixing. Bretherton's prediction was applied, using the bond number to guide a design that prevents potentially biohazardous samples from leaking from the device. We employed multi-material 3D printing technology, which allows composites with rigid and elastomeric properties to be printed as a single part. To validate the meter-mix device with a clinically relevant sample, we used urine spiked with inactivated Chlamydia trachomatis and Neisseria gonorrhoeae. A downstream nucleic acid amplification by quantitative PCR (qPCR) confirmed there was no statistically significant difference between samples metered and mixed using the standard protocol and those prepared with the meter-mix device, showing the 3D-printed device could accurately meter, mix and dispense a human urine sample without loss of nucleic acids. Although there are some limitations to 3D printing capabilities (e.g. dimension limitations related to support material used in the printing process), the advantages of customizability, modularity and rapid prototyping illustrate the utility of 3D printing for developing sample-to-device interfaces for diagnostics.

  9. Confirmation of amphetamine, methamphetamine, MDA and MDMA in urine samples using disk solid-phase extraction and gas chromatography-mass spectrometry after immunoassay screening.

    Science.gov (United States)

    Huang, Zengping; Zhang, Shaoyu

    2003-07-25

    A method using mixed phase disk solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) was developed for confirmation of amphetamine (AMP), methamphetamine (MET), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in urine samples after immunoassay screening. Disk SPE provided hydrophobic (C(18)) and strong cation-exchange (SCX) interactions. The analytes were retained on SCX functional groups in the disk and eluted with ammoniated ethyl acetate after washed with methanol. Confirmation and quantitation was exercised by selected ion monitoring using nikethamide as chromatographic standard. Recoveries of the amphetamines were between 73.0 and 104.6% with RSDs in range of 2.1-6.4% (n=3). The limits of detection were 2 ng/ml for AMP, MET and MDMA, and 4 ng/ml for MDA. Five real urine samples were tested with the method after immunoassay screening, and the results were comparable to those of traditional liquid-liquid extraction (LLE). The method was solvent-saved, simple, rapid and reliable, and the extract was cleaner than that of LLE.

  10. Comparative evaluation of seven different sample treatment approaches for large-scale multiclass sport drug testing in urine by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Domínguez-Romero, Juan C; García-Reyes, Juan F; Molina-Díaz, Antonio

    2014-09-26

    Sample preparation is a critical step in large-scale multiclass analysis such as sport drug testing. Due to the wide heterogeneity of the analytes and the complexity of the matrix, the selection of a correct sample preparation method is essential, looking for a compromise between good recoveries for most of the analytes and cleanliness of the extract. In the present work, seven sample preparation procedures based on solid-phase extraction (SPE) (with 5 different cartridges), liquid-liquid extraction (LLE) and sorbent-supported liquid extraction (SLE) were evaluated for multiclass sport drug testing in urine. The selected SPE sorbents were polymeric cartridges Agilent PLEXA™ and Oasis HLB™, mixed mode cation and anion exchange cartridges Oasis MAX™ and MCX™, and C18 cartridges. LLE was performed using tert-butyl methyl ether and SLE was carried out using Agilent Chem Elut™ cartridges. To evaluate the proposed extraction procedures, a list of 189 compounds were selected as representative from different groups of doping agents, including 34 steroids, 14 glucocorticosteroids, 24 diuretics and masking agents, 11 stimulants, 9 beta-agonist, 16 beta-blockers, 6 Selective Estrogen Receptors Modulators (SERMs), 24 narcotics and 22 other drugs of abuse/sport drugs. Blank urine samples were spiked at two levels of concentration, 2.5 and 25μgL(-1) and extracted with the different extraction protocols (n=6). The analysis of the extracts was carried out by liquid chromatography electrospray time-of-flight mass spectrometry. The use of solid-phase extraction with polymer cartridges provided high recoveries for most of the analytes tested and was found the more suitable method for this type of application given the additional advantages such as low sample and solvent consumption along with increased automation and throughput.

  11. Enantioselective analysis of pheniramine in urine by charged CD-mediated CZE provided with a fiber-based DAD and an on-line sample pretreatment by capillary ITP.

    Science.gov (United States)

    Marák, Jozef; Mikus, Peter; Maráková, Katarína; Kaniansky, Dusan; Valásková, Iva; Havránek, Emil

    2007-08-01

    Application potentialities of CZE on-line coupled with capillary ITP and DAD to the identification and determination of trace concentration levels (microg/L) of pheniramine (PHM) enantiomers and their metabolites present in complex ionic matrices of biological origin (urine) are shown. An enhanced (enantio)selectivity of the CZE separation system obtained by the addition of carboxyethyl-beta-CD (CE-beta-CD) to the carrier electrolyte provided CZE conditions for a reliable identification of similar/identical DAD spectra of structurally related compounds (PHM enantiomers and their metabolites) in clinical urine samples differing in qualitative and quantitative composition of sample matrix constituents. A high sample loadability (a 30 microL sample injection volume), partial sample clean-up (removing macroconstituents from the sample), and preconcentration of the analytes in ITP stage resulted in the decrease of concentration LOD for PHM enantiomers in urine to 5.2 and 6.8 microg/L (2.2 x 10(-8) and 2.8 x 10(-8) mol/L), without using any sample pretreatment technique. The background correction and smoothing procedure applied to the raw DAD spectra provided analytically relevant DAD spectra of PHM enantiomers and their metabolites also when they were present in urine sample (30 microL injection volumes of ten-times diluted urine sample) at a 9 x 10(-) (8) mol/L concentration. DAD spectra of PHM enantiomers present in urine samples matched their reference spectra with reasonable certainties. DAD spectra of PHM metabolites were compared with the reference spectra of PHM enantiomers and a good match was found which indicates the similarities in the structures of enantiomers and their metabolites detected in the urine samples. This fact allows performing the quantitative analyses of PHM metabolites in the urine samples by applying the calibration parameters of PHM enantiomers also for PHM metabolites and the results show the possibilities of using the ITP

  12. Analysis of vanillylmandelic and homovanillic acids in urine using solid phase sample preparation and high pressure liquid chromatography with electrochemical detection.

    Science.gov (United States)

    Bremmelgaard, A

    1985-09-01

    A rapid, simple and specific method for quantification of vanillylmandelic acid (VMA) and homovanillic acid (HVA) in urine is described. The method is suitable for routine use and may include other organic acids in human urine.

  13. Application of cloud point preconcentration and flame atomic absorption spectrometry for the determination of cadmium and zinc ions in urine, blood serum and water samples

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2013-01-01

    Full Text Available A simple, sensitive and selective cloud point extraction procedure is described for the preconcentration and atomic absorption spectrometric determination of Zn2+ and Cd2+ ions in water and biological samples, after complexation with 3,3',3",3'"-tetraindolyl (terephthaloyl dimethane (TTDM in basic medium, using Triton X-114 as nonionic surfactant. Detection limits of 3.0 and 2.0 µg L-1 and quantification limits 10.0 and 7.0 µg L-1were obtained for Zn2+ and Cd2+ ions, respectively. Relative standard deviation was 2.9 and 3.3, and enrichment factors 23.9 and 25.6, for Zn2+ and Cd2+ ions, respectively. The method enabled determination of low levels of Zn2+ and Cd2+ ions in urine, blood serum and water samples.

  14. Entering markets and bodies: increasing levels of the novel plasticizer Hexamoll® DINCH® in 24 h urine samples from the German Environmental Specimen Bank.

    Science.gov (United States)

    Schütze, André; Kolossa-Gehring, Marike; Apel, Petra; Brüning, Thomas; Koch, Holger M

    2014-03-01

    DINCH (diisononylcyclohexane-1,2-dicarboxylate) was introduced into the world market in 2002 as a non-aromatic plasticizer and phthalate substitute. We analyzed 300 urine samples (24 h voids) of the German Environmental Specimen Bank (ESB for Human tissues, ESB Hum) for specific DINCH metabolites by on-line HPLC-MS/MS with isotope dilution quantification. Urine samples of the ESB Hum were from the years 1999, 2003, 2006, 2009 and 2012, chosen to investigate the appearance and a possible trend of DINCH exposure since its market introduction. No DINCH metabolites were detected in the 1999 and 2003 samples. From 2006 on, the percentage of samples with DINCH metabolites above the LOQ increased significantly over the years (7% in 2006, 43% in 2009 and 98% in 2012). The cyclohexane-1,2-dicarboxylic acid-mono(hydroxy-isononyl) ester (OH-MINCH) was the predominant metabolite. Median (and 95th percentile) concentrations (in μg/l) increased from 0.75, p<0.001). The median (95th percentile) DINCH intake in 2012 was calculated to be 0.14 (1.07)μg/kg body weight/day which is considerably below daily intakes currently deemed tolerable. DINCH is regarded to have a preferred toxicological profile over certain anti-androgenic phthalates. The continuation of DINCH measurements in the ESB Hum and other human biomonitoring studies like the German Environmental Survey (GerES) allows tracking the development of DINCH body burdens, the distribution of exposure levels and daily intakes, providing basic data for future toxicological assessment and further epidemiological studies.

  15. Absorptive constituents and their metabolites in drug-containing urine samples from Wuzhishan miniature pigs orally administered with Buyang Huanwu decoction.

    Science.gov (United States)

    Yang, Dong-Hui; Ren, Xiang-Liang; Xu, Feng; Ma, Xiao-Qing; Liu, Guang-Xue; Li, Cang-Hai; Li, Chen; Cai, Shao-Qing

    2014-01-01

    Buyang Huanwu decoction (BYHWD), a famous traditional Chinese medicine prescription for the treatment of cerebrovascular diseases, is composed of seven commonly used Chinese herbs--Astragali Radix, Angelicae Sinensis Radix, Paeoniae Radix Rubra, Chuanxiong Rhizoma, Carthami Flos, Persicae Semen and Pheretima. To determine the main absorptive constituents and the metabolites of BYHWD in vivo, urine samples from Wuzhishan (WZS) miniature pigs orally administered with BYHWD (13.6 g crude drugs/kg) were collected to investigate the characteristic compounds. By comparing the high-performance liquid chromatography of a drug-containing urine sample with that of a drug-free sample, 17 characteristic compounds were isolated from the methanol extract of a drug-containing urine sample by column chromatography. Their structures, including 11 isoflavanoids, 2 pterocarpanoids and 4 isoflavonoids, were identified by spectroscopic means. Of the 17 compounds, 8 (1-8) were new compounds with the following structures: 3S-7,3',4'-trihydroxyisoflavan-3'-O-β-D-glucuronide (1), 3S-7,3',4'-trihydroxyisoflavan-4'-O-β-D-glucuronide (2), 3S-7,2',4'-trihydroxyisoflavan-2'-O-β-D-glucuronide (3), 3R-7,2'-dihydroxy-3',4'-dimethoxyisoflavan-2'-O-β-D-glucuronide (4), 3R-7,2'-dihydroxy-3',4'-dimethoxyisoflavan-2'-O-β-D-glucuronide-6"-methyl ester (5), 3R-7,2'-dihydroxy-3',4'-dimethoxyisoflavan-7-O-β-D-glucuronide-6"-methyl ester (6), 3R-7,2',3'-trihydroxy-4'-methoxyisoflavan-3'-O-β-D-glucuronide-6"-methyl ester (7), and 3S-7,4',5'-trihydroxy-2',3'-dimethoxyisoflavan-5'-O-β-D-glucuronide (8). Based on the possible relationship and metabolic pathways of the 17 compounds in vivo, 3R-7,2'-dihydroxy-3',4'-dimethoxyisoflavan (isomucronulatol, 11), 6aR,11aR-3-hydroxy-9,10-dimethoxypterocarpan (methylnissolin, astrapterocarpan, 13), 7,3'-dihydroxy-4'-methoxyisoflavone (calycosin, 16) and 7-hydroxy-4'-methoxyisoflavone (formononetin, 17) were thought to be the most important absorptive original

  16. Ketones urine test

    Science.gov (United States)

    Ketone bodies - urine; Urine ketones; Ketoacidosis - urine ketones test; Diabetic ketoacidosis - urine ketones test ... Urine ketones are usually measured as a "spot test." This is available in a test kit that ...

  17. Electrokinetic extraction on artificial liquid membranes of amphetamine-type stimulants from urine samples followed by high performance liquid chromatography analysis.

    Science.gov (United States)

    Seidi, Shahram; Yamini, Yadollah; Baheri, Tahmineh; Feizbakhsh, Rouhollah

    2011-07-01

    Electromembrane extraction (EME) coupled with high performance liquid chromatography and ultraviolet detection was developed for determination of amphetamine-type stimulants in human urine samples. Amphetamines migrated from 3 mL of different human urine matrices, through a thin layer of 2-nitrophenyl octyl ether (NPOE) containing 15% tris-(2-ethylhexyl) phosphate (TEHP) immobilized in the pores of a porous hollow fiber, and into a 15 μL acidic aqueous acceptor solution present inside the lumen of the fiber. Equilibrium extraction conditions were obtained after 7 min of operation. Experimental design and response surface methodology (RSM) were used for optimization of EME parameters. Under optimal conditions, amphetamines were effectively extracted with recoveries in the range of 54-70%, which corresponded to preconcentration factors in the range of 108-140. The calibration curves were investigated in the range of 0-7 μg mL(-1) and good linearity was achieved with a coefficient of estimation better than 0.991. Detection limits and inter-day precision (n=3) were less than 0.01 μg mL(-1) and 11.2%, respectively.

  18. Separation and quantitative determination of cinacalcet metabolites in urine sample using RP-HPLC after derivation with a fluorescent labeling reagent.

    Science.gov (United States)

    Farnoudian-Habibi, Amir; Jaymand, Mehdi

    2016-08-01

    In this investigation, a novel strategy for separation and quantitative determination of four metabolites of cinacalcet (M2a-Glu, M2b-Glu, M7-Gly, and M8-Gly) in human urine is suggested. The analytical assay is based on a pre-column derivation procedure of cinacalcet metabolites with 1-pyrenyldiazomethane (PDAM) as a fluorescent labeling reagent, and subsequently separation and quantitative determination with reverse-phase high-performance liquid chromatography (RP-HPLC) coupled with a fluorescence detector. Metabolites were separated on a Microsorb-MV 100-5 C18 chromatography column (250×4.6mm, 5μm) using acetate buffer (pH 3.5):methanol (30:70 v/v) as mobile phase at a flow rate of 1.0mLmin(-1). The method was fully validated in terms of linearity (r(2)>0.996; 1-10ngmL(-1)), precision (both intra-day and inter-day; RSD<6.2%), accuracy (92-110%), specificity, robustness (0.15%urine samples.

  19. Vortex-assisted liquid-liquid extraction combined with field-amplified sample injection and sweeping micellar electrokinetic chromatography for improved determination of β-blockers in human urine.

    Science.gov (United States)

    Jouyban, Abolghasem; Sorouraddin, Mohammad Hossein; Farajzadeh, Mir Ali; Somi, Mohammad Hossein; Fazeli-Bakhtiyari, Rana

    2016-01-01

    A new micellar electrokinetic chromatography (MEKC) method was developed and validated for the analysis of carvedilol and propranolol in human urine samples. In this study, vortex-assisted liquid-liquid extraction (VALLE) coupled with field-amplified sample injection and sweeping was employed for biological sample clean-up and sensitivity enhancement in MEKC. After VALLE, the urine samples were analyzed by MEKC. Tris-phosphate buffer (60mmolL(-1), pH 2.0) containing 40% (v/v) methanol was first filled into an uncoated fused-silica capillary (56cm, 50µm i.d.). The pretreated urine sample was loaded by electrokinetic injection (10kV, 250s). The stacking and separation were performed using Tris-phosphate buffer (30mmolL(-1), pH 3.0) containing 30% (v/v) methanol and 50mmolL(-1) sodium dodecyl sulfate (SDS) at -25kV. Detection was carried out at 195 and 214nm for carvedilol and propranolol, respectively. The suggested method is linear (r(2)≥0.997) over a dynamic range of 0.005-1µgmL(-1) in urine. The intra- and inter-day relative standard deviation and relative error values of the method were below 20%, which shows good precision and accuracy. Finally, this method was successfully applied to the analysis of real urine samples.

  20. MAIIA EPO SeLect-a rapid screening kit for the detection of recombinant EPO analogues in doping control: inter-laboratory prevalidation and normative study of athlete urine and plasma samples.

    Science.gov (United States)

    Dehnes, Yvette; Myrvold, Linda; Ström, Helene; Ericsson, Magnus; Hemmersbach, Peter

    2014-01-01

    Recombinant analogues of erythropoietin (EPO), epoetins, have been misused by athletes due to their performance enhancing effect since the first pharmaceutical epoetin was launched in 1987. The current methods for screening urine and plasma samples for the presence of epoetins, IEF and SAR-PAGE, have high sensitivity but are time-consuming to carry out. In an effort to ease and speed up the screening procedure for EPO, MAIIA Diagnostics has developed a combined affinity chromatography and lateral flow immunoassay, MAIIA EPO SeLect, which determines the percentage of migrated isoforms (PMI) of EPO in a sample. The reproducibility of the kit was tested by analyzing a set of negative and positive urine and plasma samples in three different laboratories. All data were analyzed with both curve fit parameters from the individual assay runs, and with lot-specific predefined curve calibration. To get a measure of endogenous variation, a normative study with athlete urine and plasma samples was conducted. The average intra-laboratory variation was 6.7% while the inter-laboratory variation for all samples was calculated to 8.8%. The athlete samples yielded an average PMI and standard deviation of 71.4 ± 7.7 for urine and 83.1 ± 10.2 for plasma, respectively. There were no signs of deviating results from tested effort urines. The results also support the use of predefined curve parameters.

  1. Occurrence of artificial sweeteners in human liver and paired blood and urine samples from adults in Tianjin, China and their implications for human exposure.

    Science.gov (United States)

    Zhang, Tao; Gan, Zhiwei; Gao, Chuanzi; Ma, Ling; Li, Yanxi; Li, Xiao; Sun, Hongwen

    2016-09-14

    In this study, acesulfame (ACE), saccharin (SAC) and cyclamate (CYC) were found in all paired urine and blood samples collected from healthy adults, with mean values of 4070, 918 and 628 ng mL(-1), respectively, in urine and 9.03, 20.4 and 0.72 ng mL(-1), respectively, in blood. SAC (mean: 84.4 ng g(-1)) and CYC (4.29 ng g(-1)) were detectable in all liver samples collected from liver cancer patients, while ACE was less frequently detected. Aspartame (ASP) was not found in any analyzed human sample, which can be explained by the fact that this chemical metabolized rapidly in the human body. Among all adults, significantly positive correlations between SAC and CYC levels were observed (p < 0.001), regardless of human matrices. Nevertheless, no significant correlations between concentrations of SAC (or CYC) and ACE were found in any of the human matrices. Our results suggest that human exposure to SAC and CYC is related, whereas ACE originates from a discrete source. Females (or young adults) were exposed to higher levels of SAC and CYC than males (or elderly). The mean renal clearance of SAC was 730 mL per day per kg in adults, which was significantly (p < 0.001) lower than those for CYC (10 800 mL per day per kg) and ACE (10 300 mL per day per kg). The average total daily intake of SAC and ACE was 9.27 and 33.8 μg per kg bw per day, respectively.

  2. Correlation of spot urine protein-creatinine ratio with 24-hour urinary protein in type 2 diabetes mellitus patients: A cross sectional study

    Directory of Open Access Journals (Sweden)

    Satish Basanagouda Biradar

    2011-01-01

    Full Text Available Background: Diabetic nephropathy is the major cause for chronic renal failure (CRF and proteinuria is an independent risk factor for end stage renal disease. Hence, early identification and quantification of proteinuria is of prime importance in the diagnosis and management. Methods: This study was conducted amongst 42 diabetic subjects from HSK hospital, Bagalkot. Twenty four-hour urine protein and random urine protein to creatinine ratio (P:C was determined. Pearson′s correlation, sensitivity, specificity, positive and negative predictive values were determined using 24-hour urinary protein as a gold standard for spot urine P:C ratio. ROC curve and area under curve was also determined using SPSS (11.5 software. All the results were expressed in mean±SD. Results: Forty two diabetes mellitus patients participated in this study. The average of 24 hour urinary protein was 1.6 ± 1.7 gm/day. The spot urine P:C ratio was 1.27 ± 1.55. There was a positive correlation between 24 hours urinary protein and spot urine P:C ratio (r = 0.925, p < 0.0001. The area under the ROC curve for urine P:C ratio at various cutoff was 0.947 (95% confidence interval: 0.831-0.992, p < 0.0001. The sensitivity and specificity was 80.65% and 100% respectively at P:C ratio cutoff of 0.3. Conclusions: The random urine P:C ratio predicts the amount of 24-hour urinary protein excretion with high accuracy. Hence it can be used as a faster diagnostic substitute for 24-hour urinary protein estimation.

  3. Method development for cortisol and cortisone by micellar liquid chromatography using sodium dodecyl sulphate: application to urine samples of rugby players.

    Science.gov (United States)

    Izquierdo-Hornillos, R; Gonzalo-Lumbreras, R; Santos-Montes, A

    2005-01-01

    The chromatographic behavior of cortisol and cortisone using a micellar medium of sodium dodecyl sulphate (SDS) as surfactant, a Hypersil C18 (150- x 3.2-mm i.d., 5 microm) column, a flow rate of 0.5 mL/min, and UV absorbance detection at 245 nm is described. The effect of several organic modifiers and the surfactant concentration on the separation is studied. A mobile phase of 18 mM SDS and 8.3% tetrahydrofuran allows for the separation of cortisol and cortisone up to baseline. These results are also achieved by applying a bivariant optimization method. The proposed method is sensitive, reproducible, and selective. In addition, it is less expensive than conventional high-performance liquid chromatography methods for cortisol and cortisone. The method is applied to the determination of cortisol and cortisone in urine samples of rugby players before and after stress for doping control purposes.

  4. Detection of high-level aminoglycoside resistant pattern of Enterococci isolated from urine samples at a tertiary care hospital in Bengaluru

    Directory of Open Access Journals (Sweden)

    Smeeta Huidrom

    2016-01-01

    Full Text Available Aims: Enterococcus species are major nosocomial pathogens and they most commonly cause urinary tract infections (UTIs, exhibiting vancomycin and high-level aminoglycoside resistance (HLAR with increasing frequency, resulting in high mortality of patients with serious enterococcal infections. Detection of resistance is thus of paramount importance. The present study aims to detect and determine the HLAR pattern of Enterococci isolated from urine samples of patients diagnosed with UTI at our hospital. Materials and Methods: This study was carried out at a tertiary care hospital in Bengaluru for a period of 1 year from January 2013 to December 2013. A total of 105 enterococcal strains were isolated from urine samples and speciated as per the scheme of Facklam and Collins. Antibiotic susceptibility was determined for various drugs by Kirby–Bauer disc diffusion method. The results were interpreted as per the Clinical and Laboratory Standards Institute (CLSI guidelines. Results: Ninety-three of the 105 (88.6% isolates showed high-level resistance to gentamicin and/or streptomycin. Combined resistance to both the aminoglycosides, high level gentamicin and streptomycin (HLAR, was seen only in Enterococcus faecalis 20/105 (19.04%. Of the two isolates of Enterococcus faecium, 1 (50% was seen to be resistant to high level gentamicin. The HLAR E. faecalis and E. faecium isolates also showed concordant resistance to multiple antibiotics including vancomycin. Conclusion: This study highlights the need to screen for HLAR in patients suffering from enterococcal infections. Routine screening for HLAR is important to limit the spread of resistance and to have a surveillance program.

  5. Analytical investigations of toxic p-phenylenediamine (PPD) levels in clinical urine samples with special focus on MALDI-MS/MS.

    Science.gov (United States)

    Hooff, Gero P; van Huizen, Nick A; Meesters, Roland J W; Zijlstra, Eduard E; Abdelraheem, Mohamed; Abdelraheem, Waleed; Hamdouk, Mohamed; Lindemans, Jan; Luider, Theo M

    2011-01-01

    Para-phenylenediamine (PPD) is a common chromophoric ingredient in oxidative hair-dyes. In some African countries like Sudan, Egypt and Morocco but also in India this chemical is used alone or in combination with colouring extracts like Henna for dyeing of the hair or the skin. Excessive dermal exposure to PPD mainly leads to the N-mono- and N,N'-diacetylated products (MAPPD, DAPPD) by N-acetyltransferase 1 and 2 (NAT1 and 2) catalyzed reactions. Metabolites and PPD are mainly excreted via renal clearance. Despite a low risk of intoxication when used in due form, there are numerous cases of acute intoxication in those countries every year. At the ENT Hospital - Khartoum (Sudan) alone more than 300 cases are reported every year (~10% fatal), mostly caused by either an accidental or intended (suicidal) high systemic exposure to pure PPD. Intoxication leads to a severe clinical syndrome including laryngeal edema, rhabdomyolysis and subsequent renal failure, neurotoxicity and acute toxic hepatitis. To date, there is no defined clinical treatment or antidote available and treatment is largely supportive. Herein, we show the development of a quick on-site identification assay to facilitate differential diagnosis in the clinic and, more importantly, the implementation of an advanced analytical platform for future in-depth investigations of PPD intoxication and metabolism is described. The current work shows a sensitive (~25 µM) wet chemistry assay, a validated MALDI-MS/MS and HPLC-UV assay for the determination of PPD and its metabolites in human urine. We show the feasibility of the methods for measuring PPD over a range of 50-1000 µM. The validation criteria included linearity, lower limit of quantification (LLOQ), accuracy and precision, recovery and stability. Finally, PPD concentrations were determined in clinical urine samples of cases of acute intoxication and the applied technique was expanded to identify MAPPD and DAPPD in the identical samples.

  6. Analytical investigations of toxic p-phenylenediamine (PPD levels in clinical urine samples with special focus on MALDI-MS/MS.

    Directory of Open Access Journals (Sweden)

    Gero P Hooff

    Full Text Available Para-phenylenediamine (PPD is a common chromophoric ingredient in oxidative hair-dyes. In some African countries like Sudan, Egypt and Morocco but also in India this chemical is used alone or in combination with colouring extracts like Henna for dyeing of the hair or the skin. Excessive dermal exposure to PPD mainly leads to the N-mono- and N,N'-diacetylated products (MAPPD, DAPPD by N-acetyltransferase 1 and 2 (NAT1 and 2 catalyzed reactions. Metabolites and PPD are mainly excreted via renal clearance. Despite a low risk of intoxication when used in due form, there are numerous cases of acute intoxication in those countries every year. At the ENT Hospital - Khartoum (Sudan alone more than 300 cases are reported every year (~10% fatal, mostly caused by either an accidental or intended (suicidal high systemic exposure to pure PPD. Intoxication leads to a severe clinical syndrome including laryngeal edema, rhabdomyolysis and subsequent renal failure, neurotoxicity and acute toxic hepatitis. To date, there is no defined clinical treatment or antidote available and treatment is largely supportive. Herein, we show the development of a quick on-site identification assay to facilitate differential diagnosis in the clinic and, more importantly, the implementation of an advanced analytical platform for future in-depth investigations of PPD intoxication and metabolism is described. The current work shows a sensitive (~25 µM wet chemistry assay, a validated MALDI-MS/MS and HPLC-UV assay for the determination of PPD and its metabolites in human urine. We show the feasibility of the methods for measuring PPD over a range of 50-1000 µM. The validation criteria included linearity, lower limit of quantification (LLOQ, accuracy and precision, recovery and stability. Finally, PPD concentrations were determined in clinical urine samples of cases of acute intoxication and the applied technique was expanded to identify MAPPD and DAPPD in the identical samples.

  7. Evaluation of ephedrine, pseudoephedrine and phenylpropanolamine concentrations in human urine samples and a comparison of the specificity of DRI amphetamines and Abuscreen online (KIMS) amphetamines screening immunoassays.

    Science.gov (United States)

    Stout, Peter R; Klette, Kevin L; Horn, Carl K

    2004-01-01

    The purpose of this study was to evaluate the ability of two amphetamine class screening reagents to exclude ephedrine (EPH), pseudoephedrine (PSEPH), and phenylpropanolamine (PPA) from falsely producing positive immunoassay screening results. The study also sought to characterize the prevalence and concentration distributions of EPH, PSEPH, and PPA in samples that produced positive amphetamine screening results. Approximately 27,400 randomly collected human urine samples from Navy and Marine Corps members were simultaneously screened for amphetamines using the DRI and Abuscreen online immunoassays at a cutoff concentration of 500 ng/mL. All samples that screened positive were confirmed for amphetamine (AMP), methamphetamine (MTH), 3,4-Methylenedioxyamphetamine (MDA), 3,4-Methylenedioxymethamphetamine (MDMA), EPH, PSEPH, and PPA by gas chromatography/mass spectrometry (GC/MS). The DRI AMP immunoassay identified 1,104 presumptive amphetamine positive samples, of which only 1.99% confirmed positive for the presence of AMP, MTH, MDA, or MDMA. In contrast, the online AMP reagent identified 317 presumptive amphetamine positives with a confirmation rate for AMP, MTH, MDA, or MDMA of 7.94%. The presence of EPH, PSEPH, or PPA was confirmed in 833 of the 1,104 samples that failed to confirm positive for AMP, MTH, MDA, or MDMA; all of the 833 samples contained PSEPH. When compared to the entire screened sample set, PSEPH was present in approximately 3%, EPH in 0.9%, and PPA in 0.8% of the samples. The results indicate that cross reactivities for EPH, PSEPH, and PPA are greater than reported by the manufacturer of these reagents. The distribution of concentrations indicates that very large concentrations of EPH, PSEPH, and PPA are common.

  8. High performance liquid chromatographic determination of ultra traces of two tricyclic antidepressant drugs imipramine and trimipramine in urine samples after their dispersive liquid-liquid microextraction coupled with response surface optimization.

    Science.gov (United States)

    Shamsipur, Mojtaba; Mirmohammadi, Mehrosadat

    2014-11-01

    Dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography by ultraviolet detection (HPLC-UV) as a fast and inexpensive technique was applied to the determination of imipramine and trimipramine in urine samples. Response surface methodology (RSM) was used for multivariate optimization of the effects of seven different parameters influencing the extraction efficiency of the proposed method. Under optimized experimental conditions, the enrichment factors and extraction recoveries were between 161.7-186.7 and 97-112%, respectively. The linear range and limit of detection for both analytes found to be 5-100ng mL(-1) and 0.6ng mL(-1), respectively. The relative standard deviations for 5ng mL(-1) of the drugs in urine samples were in the range of 5.1-6.1 (n=5). The developed method was successfully applied to real urine sample analyses.

  9. Rapid Molecular Detection of Zika Virus in Acute-Phase Urine Samples Using the Recombinase Polymerase Amplification Assay

    Science.gov (United States)

    Abd El Wahed, Ahmed; Sanabani, Sabri Saeed; Faye, Oumar; Pessôa, Rodrigo; Patriota, João Veras; Giorgi, Ricardo Rodrigues; Patel, Pranav; Böhlken-Fascher, Susanne; Landt, Olfert; Niedrig, Matthias; Zanotto, Paolo Marinho de Andrade; Czerny, Claus Peter; Sall, Amadou A.; Weidmann, Manfred

    2017-01-01

    Background: Currently the detection of Zika virus (ZIKV) in patient samples is done by real-time RT-PCR. Samples collected from rural area are sent to highly equipped laboratories for screening. A rapid point-of-care test is needed to detect the virus, especially at low resource settings. Methodology/Principal Findings: In this report, we describe the development of a reverse transcription isothermal recombinase polymerase amplification (RT-RPA) assay for the identification of ZIKV. RT-RPA assay was portable, sensitive (21 RNA molecules), and rapid (3-15 minutes). No cross-reactivity was detected to other flaviviruses, alphaviruses and arboviruses. Compared to real-time RT-PCR, the diagnostic sensitivity was 92%, while the specificity was 100%. Conclusions/Significance: The developed assay is a promising platform for rapid point of need detection of ZIKV in low resource settings and elsewhere (e.g. during mass gathering). PMID:28239513

  10. Urine culture - catheterized specimen

    Science.gov (United States)

    Culture - urine - catheterized specimen; Urine culture - catheterization; Catheterized urine specimen culture ... urinary tract infections may be found in the culture. This is called a contaminant. You may not ...

  11. Thin layer chromatography of camel urine

    Directory of Open Access Journals (Sweden)

    Tarig Hab,

    2011-06-01

    Full Text Available General screening of 10 camel urine samples was carried out to determine the most common constituent of camel urine. Samples used were crude, ethanolic and chlorofermic extracts and compared with their lyophilysed urine. The study revealed the presence of alkaloids and triterpene. The objectives of this investigation are to verify camel urine major chemical constituents which are extremely valuable information for detecting new drugs of natural origin.

  12. Highly sensitive and selective determination of pyrazinamide at poly-L-methionine/reduced graphene oxide modified electrode by differential pulse voltammetry in human blood plasma and urine samples.

    Science.gov (United States)

    Cheemalapati, Srikanth; Devadas, Balamurugan; Chen, Shen-Ming

    2014-03-15

    In this current study we used electrochemically active film which contains poly-L-methionine (PMET) and electrochemically reduced graphene oxide (ERGO) on glassy carbon electrode (GCE) for pyrazinamide (PZM) detection. The electrocatalytic response of analyte at PMET/ERGO/GCE film was measured using both cyclic voltammetry (CV) and differential pulse voltammetry (DPV). In addition, electrochemical impedance studies revealed that the smaller R(ct) value observed at PMET/ERGO film modified GCE which authenticates its good conductivity and faster electron transfer rate. The prepared PMET/ERGO/GCE film exhibits excellent DPV response towards PZM and the reduction peak current increased linearly with respect to PZM concentration in the linear range between 0.4 μM to 1129 μM with a sensitivity of 0.266 μA μM(-1) cm(-2). Real sample studies were carried out in human blood plasma and urine samples, which offered good recovery and revealed the promising practicality of the sensor for PZM detection. The proposed sensor displayed a good selectivity, repeatability, sensitivity with appreciable consistency and good reproducibility. In addition, the proposed electrochemical sensor showed good results towards the commercial pharmaceutical PZM samples.

  13. Monitoring Intravenous Abuse of Methadone or Buprenorphine in Opiate Maintenance Treatment (OMT): A Simple and Fast LC-MS-MS Method for the Detection of Disaccharides in Urine Samples.

    Science.gov (United States)

    Jungen, Hilke; Andresen-Streichert, Hilke; Müller, Alexander; Iwersen-Bergmann, Stefanie

    2017-01-01

    The detection of disaccharides in urine is under investigation to act as a marker for intravenous abuse of disaccharide formulations, like liquid methadone with syrup (sucrose), methadone tablets (lactose and sucrose), or buprenorphine tablets (lactose). As the detection time in urine has not yet been investigated and a routine method for detecting disaccharides is still lacking, a study was performed to estimate the window of detection in urine after intravenous consumption of disaccharides. Furthermore, an analytical LC-MSMS method for the quantification of sucrose and lactose in urine was validated. The method was applied to urine samples of intravenous substitute consumers, with urine being sampled before intravenous use of substitutes and approximately 30 minutes later. Twenty users provided information regarding their most recent prior intravenous consumption. Disaccharides were detectable in all 20 urine samples about 30 minutes after consumption. A cut off for both disaccharides of 40mg/L was used. Based on these conditions 81% of the persons who consumed in a time frame of 24 hours ago showed positive results for disaccharides. The study showed that the validated LC-MSMS method with an easy and fast workup is usable for daily routine in the laboratory. It might be helpful for methadone and buprenorphine prescribing physicians to check whether the opiate maintenance treatment patient takes his or her substitution medicines orally as intended, or continues with intravenous misuse by injecting substitution medicines instead of heroin. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  14. Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Fan, Wenying; He, Man; You, Linna; Zhu, Xuewei; Chen, Beibei; Hu, Bin

    2016-04-22

    Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37 μg L(-1), and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5 μg L(-1) and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine

  15. Urine Tests (For Parents)

    Science.gov (United States)

    ... TOPIC Vesicoureteral Reflux (VUR) Blood in the Urine (Hematuria) Urine Test: Creatinine Urine Test: Microalbumin-to-Creatinine ... Video) Urinary Tract Infections Blood in the Urine (Hematuria) Kidneys and Urinary Tract Contact Us Print Resources ...

  16. Urination - difficulty with flow

    Science.gov (United States)

    ... common cause is infection of the prostate or urinary tract. Symptoms of a possible infection include: Burning or pain with urination Frequent urination Cloudy urine Sense of urgency (strong, sudden urge to urinate) The problem can ...

  17. Behavior of phenols and phenoxyacids on a bisphenol-A imprinted polymer. Application for selective solid-phase extraction from water and urine samples.

    Science.gov (United States)

    Herrero-Hernández, Eliseo; Carabias-Martínez, Rita; Rodríguez-Gonzalo, Encarnacion

    2011-01-01

    A molecularly imprinted polymer (MIP), obtained by precipitation polymerisation with 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate as cross-linker, and bisphenol-A (BPA) as template, was prepared. The binding site configuration of the BPA-MIP was examined using Scatchard analysis. Moreover, the behaviour of the BPA-MIP for the extraction of several phenolic compounds (bisphenol-A, bisphenol-F, 4-nitrophenol, 3-methyl-4-nitrophenol) and phenoxyacid herbicides such as 2,4-D, 2,4,5-T and 2,4,5-TP has been studied in organic and aqueous media in the presence of other pesticides in common use. It was possible to carry out the selective preconcentration of the target analytes from the organic medium with recoveries of higher than 70%. In an aqueous medium, hydrophobic interactions were found to exert a remarkably non-specific contribution to the overall binding process. Several parameters affecting the extraction efficiency of the BPA-MIP were evaluated to achieve the selective preconcentration of phenols and phenoxyacids from aqueous samples. The possibility of using the BPA-MIP as a selective sorbent to preconcentrate these compounds from other samples such as urine and river water was also explored.

  18. Screening determination of four amphetamine-type drugs in street-grade illegal tablets and urine samples by portable capillary electrophoresis with contactless conductivity detection.

    Science.gov (United States)

    Nguyen, Thi Anh Huong; Pham, Thi Ngoc Mai; Ta, Thi Thao; Nguyen, Xuan Truong; Nguyen, Thi Lien; Le, Thi Hong Hao; Koenka, Israel Joel; Sáiz, Jorge; Hauser, Peter C; Mai, Thanh Duc

    2015-12-01

    A simple and inexpensive method for the identification of four substituted amphetamines, namely, 3,4-methylenedioxy methamphetamine (MDMA), methamphetamine (MA), 3,4-methylenedioxy amphetamine (MDA) and 3,4-methylenedioxy-N-ethylamphetamine (MDEA) was developed using an in-house constructed semi-automated portable capillary electrophoresis instrument (CE) with capacitively coupled contactless conductivity detection (C(4)D). Arginine 10mM adjusted to pH4.5 with acetic acid was found to be the optimal background electrolyte for the CE-C(4)D determination of these compounds. The best detection limits achieved with and without a sample preconcentration process were 10ppb and 500ppb, respectively. Substituted amphetamines were found in different seized illicit club drug tablets and urine samples collected from different suspected users. Good agreement between results from CE-C(4)D and those with the confirmation method (GC-MS) was achieved, with correlation coefficients for the two pairs of data of more than 0.99.

  19. Graphene oxide assisted electromembrane extraction with gas chromatography for the determination of methamphetamine as a model analyte in hair and urine samples.

    Science.gov (United States)

    Bagheri, Hasan; Zavareh, Alireza Fakhari; Koruni, Mohammad Hossein

    2016-03-01

    In the present study, graphene oxide reinforced two-phase electromembrane extraction (EME) coupled with gas chromatography was applied for the determination of methamphetamine as a model analyte in biological samples. The presence of graphene oxide in the hollow fiber wall can increase the effective surface area, interactions with analyte and polarity of support liquid membrane that leads to an enhancement in the analyte migration. To investigate the influence of the presence of graphene oxide in the support liquid membrane on the extraction efficiency, a comparative study was performed between graphene oxide and graphene oxide/EME methods. The extraction parameters such as type of organic solvent, pH of the donor phase, stirring speed, time, voltage, salt addition and the concentration of graphene oxide were optimized. Under the optimum conditions, the proposed microextraction technique provided low limit of detection (2.4 ng/mL), high preconcentration factor (195-198) and high relative recovery (95-98.5%). Finally, the method was successfully employed for the determination of methamphetamine in urine and hair samples.

  20. Behavior of Phenols and Phenoxyacids on a Bisphenol-A Imprinted Polymer. Application for Selective Solid-Phase Extraction from Water and Urine Samples

    Directory of Open Access Journals (Sweden)

    Eliseo Herrero-Hernández

    2011-05-01

    Full Text Available A molecularly imprinted polymer (MIP, obtained by precipitation polymerisation with 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate as cross-linker, and bisphenol-A (BPA as template, was prepared. The binding site configuration of the BPA-MIP was examined using Scatchard analysis. Moreover, the behaviour of the BPA-MIP for the extraction of several phenolic compounds (bisphenol-A, bisphenol-F, 4-nitrophenol, 3-methyl-4-nitrophenol and phenoxyacid herbicides such as 2,4-D, 2,4,5-T and 2,4,5-TP has been studied in organic and aqueous media in the presence of other pesticides in common use. It was possible to carry out the selective preconcentration of the target analytes from the organic medium with recoveries of higher than 70%. In an aqueous medium, hydrophobic interactions were found to exert a remarkably non-specific contribution to the overall binding process. Several parameters affecting the extraction efficiency of the BPA-MIP were evaluated to achieve the selective preconcentration of phenols and phenoxyacids from aqueous samples. The possibility of using the BPA-MIP as a selective sorbent to preconcentrate these compounds from other samples such as urine and river water was also explored.

  1. Determination of γ-hydroxybutyrate (GHB), β-hydroxybutyrate (BHB), pregabalin, 1,4-butane-diol (1,4BD) and γ-butyrolactone (GBL) in whole blood and urine samples by UPLC-MSMS.

    Science.gov (United States)

    Dahl, Sandra Rinne; Olsen, Kirsten Midtbøen; Strand, Dag Helge

    2012-02-15

    The demand of high throughput methods for the determination of gamma-hydroxybutyrate (GHB) and its precursors gamma-butyrolactone (GBL) and 1,4-butane-diol (1,4BD) as well as for pregabalin is increasing. Here we present two analytical methods using ultra-high pressure liquid chromatography (UPLC) and tandem mass spectrometric (MS/MS) detection for the determination of GHB, beta-hydroxybutyrate (BHB), pregabalin, 1,4BD and GBL in whole blood and urine. Using the 96-well formate, the whole blood method is a simple high-throughput method suitable for screening of large sample amounts. With an easy sample preparation for urine including only dilution and filtration of the sample, the method is suitable for fast screening of urine samples. Both methods showed acceptable linearity, acceptable limits of detection, and limits of quantification. The within-day and between-day precisions of all analytes were lower than 10% RSD. The analytes were extracted from matrices with recoveries near 100%, and no major matrix effects were observed. Both methods have been used as routine screening analyses of whole blood and urine samples since January 2010.

  2. Quantitative chiral and achiral determination of ketamine and its metabolites by LC-MS/MS in human serum, urine and fecal samples.

    Science.gov (United States)

    Hasan, Mahmoud; Hofstetter, Robert; Fassauer, Georg M; Link, Andreas; Siegmund, Werner; Oswald, Stefan

    2017-05-30

    Ketamine (KET) is a widely used anesthetic drug which is metabolized by CYP450 enzymes to norketamine (n-KET), dehydronorketamine (DHNK), hydroxynorketamine (HNK) and hydroxyketamine (HK). Ketamine is a chiral compound and S-ketamine is known to be the more potent enantiomer. Here, we present the development and validation of three LC-MS/MS assays; the first for the quantification of racemic KET, n-KET and DHNK in human serum, urine and feces; the second for the separation and quantification of the S- and R-enantiomers of KET, n-KET and DHNK, and the third for separation and quantification of 2S,6S-hydroxynorketamine (2S,6S-HNK) and 2R,6R-hydroxynorketamine (2R,6R-HNK) in serum and urine with the ability to separate and detect 10 additional hydroxylated norketamine metabolites of racemic ketamine. Sample preparation was done by liquid-liquid extraction using methyl tert-butyl ether. For achiral determination of KET and its metabolites, an isocratic elution with ammonium acetate (pH 3.8; 5mM) and acetonitrile on a C18 column was performed. For the separation of S- and R-enantiomers of KET, n-KET and DHNK, a gradient elution was applied using a mobile phase of ammonium acetate (pH 7.5; 10mM) and isopropanol on the CHIRAL-AGP(®) column. The enantioselective separation of the HNK metabolites was done on the chiral column Lux(®)-Amylose-2 with a gradient method using ammonium acetate (pH 9; 5mM) and a mixture of isopropanol and acetonitrile (4:1). The mass spectrometric detection monitored for each analyte 2-3 mass/charge transitions. D4-ketamine and D4-n-KET were used as internal standards. The assays were successfully validated according to current bioanalytical guidelines and applied to a pilot study in one healthy volunteer. Compared to previously published methods, our assays have superior analytical features such as a lower amount of required matrix, faster sample preparation, shorter analytical run time and higher sensitivity (LLOQ up to 0.1ng/ml). Moreover

  3. Development and validation of a rapid turboflow LC-MS/MS method for the quantification of LSD and 2-oxo-3-hydroxy LSD in serum and urine samples of emergency toxicological cases.

    Science.gov (United States)

    Dolder, Patrick C; Liechti, Matthias E; Rentsch, Katharina M

    2015-02-01

    Lysergic acid diethylamide (LSD) is a widely used recreational drug. The aim of the present study is to develop a quantitative turboflow LC-MS/MS method that can be used for rapid quantification of LSD and its main metabolite 2-oxo-3-hydroxy LSD (O-H-LSD) in serum and urine in emergency toxicological cases without time-consuming extraction steps. The method was developed on an ion-trap LC-MS/MS instrument coupled to a turbulent-flow extraction system. The validation data showed no significant matrix effects and no ion suppression has been observed in serum and urine. Mean intraday accuracy and precision for LSD were 101 and 6.84%, in urine samples and 97.40 and 5.89% in serum, respectively. For O-H-LSD, the respective values were 97.50 and 4.99% in urine and 107 and 4.70% in serum. Mean interday accuracy and precision for LSD were 100 and 8.26% in urine and 101 and 6.56% in serum, respectively. For O-H-LSD, the respective values were 101 and 8.11% in urine and 99.8 and 8.35% in serum, respectively. The lower limit of quantification for LSD was determined to be 0.1 ng/ml. LSD concentrations in serum were expected to be up to 8 ng/ml. 2-Oxo-3-hydroxy LSD concentrations in urine up to 250 ng/ml. The new method was accurate and precise in the range of expected serum and urine concentrations in patients with a suspected LSD intoxication. Until now, the method has been applied in five cases with suspected LSD intoxication where the intake of the drug has been verified four times with LSD concentrations in serum in the range of 1.80-14.70 ng/ml and once with a LSD concentration of 1.25 ng/ml in urine. In serum of two patients, the O-H-LSD concentration was determined to be 0.99 and 0.45 ng/ml. In the urine of a third patient, the O-H-LSD concentration was 9.70 ng/ml.

  4. Efeitos agudos do exercício físico prolongado: avaliação após ultramaratona de 24 horas Acute effects of prolonged physical exercise: evaluation after a twenty-four-hour ultramarathon

    Directory of Open Access Journals (Sweden)

    Daniela Guinther Passaglia

    2012-01-01

    Full Text Available FUNDAMENTO: As consequências e os riscos do exercício físico contínuo por períodos prolongados não estão esclarecidos. OBJETIVO: Avaliar os efeitos do exercício prolongado em participantes de uma ultramaratona de 24 horas. MÉTODOS: Vinte corredores foram selecionados para avaliação, um dia antes e imediatamente após a prova em que os corredores devem percorrer a maior distância em 24 horas. Foram obtidos dados clínicos, laboratoriais e ecocardiográficos. RESULTADOS: A distância média percorrida foi de 140,3 ± 18,7 km. Os corredores apresentaram redução do peso corpóreo (p BACKGROUND: The consequences and risks of prolonged physical exercise are not well established. OBJECTIVE: To evaluate the effects of prolonged physical exercise on the participants of a 24-hour ultramarathon race. METHODS: Twenty male runners were selected for evaluation a day before and immediately after the race, where the athletes had to cover the most distance in 24 hours. Clinical, laboratory and echocardiographic data were obtained at both evaluations. RESULTS: Mean distance covered was 140.3 ± 18.7 km. Runners showed weight loss (p < 0.001 and decrease in systolic (p < 0.001 and diastolic (p = 0.004 blood pressure. Hematological changes were compatible with the physiological stress. Plasma levels of creatine phosphokinase strikingly increased post-race (163.4 ± 56.8 vs. 2978.4 ± 1921.9 U/L; p < 0.001 and was inversely correlated with distance covered: those who covered the longest distances showed the lowest CPK levels (Pearson r = 0.69, p = 0.02. After the race, 2 runners showed a slight increase in Troponin levels. One of them also had simultaneous decrease in left ventricular ejection fraction (coronary artery disease was subsequently ruled out. Basal echocardiography assessment had shown LV hypertrophy in one and increased left atrial volume in five runners. After the race, there was a decrease in E/A ratio (p < 0.01. CONCLUSION: Prolonged physical exercise is associated with metabolic and cardiovascular alterations. Cardiac abnormalities found in our study suggest that cardiac fatigue may occur in this specific race modality. The long-term effect of these alterations, while maintaining the routine practice of prolonged strenuous physical activity, is still unknown.

  5. Efeitos agudos do exercício físico prolongado: avaliação após ultramaratona de 24 horas Acute effects of prolonged physical exercise: evaluation after a twenty-four-hour ultramarathon

    Directory of Open Access Journals (Sweden)

    Daniela Guinther Passaglia

    2013-01-01

    Full Text Available FUNDAMENTO: As consequências e os riscos do exercício físico contínuo por períodos prolongados não estão esclarecidos. OBJETIVO: Avaliar os efeitos do exercício prolongado em participantes de uma ultramaratona de 24 horas. MÉTODOS: Vinte corredores foram selecionados para avaliação, um dia antes e imediatamente após a prova em que os corredores devem percorrer a maior distância em 24 horas. Foram obtidos dados clínicos, laboratoriais e ecocardiográficos. RESULTADOS: A distância média percorrida foi de 140,3 ± 18,7 km. Os corredores apresentaram redução do peso corpóreo (p BACKGROUND: The consequences and risks of prolonged physical exercise are not well established. OBJECTIVE: To evaluate the effects of prolonged physical exercise on the participants of a 24-hour ultramarathon race. METHODS: Twenty male runners were selected for evaluation a day before and immediately after the race, where the athletes had to cover the most distance in 24 hours. Clinical, laboratory and echocardiographic data were obtained at both evaluations. RESULTS: Mean distance covered was 140.3 ± 18.7 km. Runners showed weight loss (p < 0.001 and decrease in systolic (p < 0.001 and diastolic (p = 0.004 blood pressure. Hematological changes were compatible with the physiological stress. Plasma levels of creatine phosphokinase strikingly increased post-race (163.4 ± 56.8 vs. 2978.4 ± 1921.9 U/L; p < 0.001 and was inversely correlated with distance covered: those who covered the longest distances showed the lowest CPK levels (Pearson r = 0.69, p = 0.02. After the race, 2 runners showed a slight increase in Troponin levels. One of them also had simultaneous decrease in left ventricular ejection fraction (coronary artery disease was subsequently ruled out. Basal echocardiography assessment had shown LV hypertrophy in one and increased left atrial volume in five runners. After the race, there was a decrease in E/A ratio (p < 0.01. CONCLUSION: Prolonged physical exercise is associated with metabolic and cardiovascular alterations. Cardiac abnormalities found in our study suggest that cardiac fatigue may occur in this specific race modality. The long-term effect of these alterations, while maintaining the routine practice of prolonged strenuous physical activity, is still unknown.

  6. Monitorização eletrocardiográfica ambulatorial por 24-horas em cães com cardiomiopatia dilatada idiopática Twenty-four-hour ambulatory electrocardiographic monitoring in dogs with idiopathic dilated cardiomyopathy

    Directory of Open Access Journals (Sweden)

    F.L. Yamaki

    2007-12-01

    Full Text Available Caracterizou-se monitorização eletrocardiográfica ambulatorial por 24 horas (ou monitorização Holter em cães com cardiomiopatia dilatada idiopática, visando principalmente à detecção de arritmias ventriculares não detectadas pela eletrocardiografia convencional (de repouso. Para tanto, avaliaram-se 40 pacientes com diagnóstico de cardiomiopatia dilatada idiopática, por meio de exame físico e mensuração indireta da pressão arterial, além de exames eletrocardiográfico, ecocardiográfico, radiográfico de tórax e da monitorização Holter. Extra-sístoles ventriculares foram detectadas, por monitorização Holter, em 97,5% dos animais e taquicardia ventricular, em 45%. Não houve correlação entre o número de extra-sístoles ventriculares e a fração de encurtamento. Considerando as manifestações clínicas, apenas houve associação entre presença de taquicardia ventricular e histórico de síncopes. Conclui-se que a incidência de arritmias ventriculares em cães com cardiomiopatia dilatada idiopática é bastante alta, sendo a taquicardia ventricular relativamente freqüente, ocorrendo mais sob a forma não sustentada.This study aimed to characterize 24-hour ambulatory electrocardiographic monitoring (Holter monitoring in dogs with idiopathic dilated cardiomyopathy. Physical examination and indirect (Doppler blood pressure measurement, and also electrocardiography, thoracic radiography, echocardiography, and 24-hour ambulatory electrocardiographic exams were performed in 40 dogs with idiopathic dilated cardiomyopathy. Ventricular extrasystoles were detected in 97.5% of the animals, and ventricular tachycardia in 45%. No correlation between the number of ventricular extrasystoles and the shortening fraction was observed. Concerning the clinical symptoms, there was only association between the presence of ventricular tachycardia and past report of syncope. It was concluded that the incidence of ventricular arrhythmias is high in dogs with dilated cardiomyopathy, being ventricular tachycardia, mostly non-sustained, relatively frequent.

  7. Twenty Four-Hour Exposure to a 0.12 THz Electromagnetic Field Does Not Affect the Genotoxicity, Morphological Changes, or Expression of Heat Shock Protein in HCE-T Cells

    Science.gov (United States)

    Koyama, Shin; Narita, Eijiro; Shimizu, Yoko; Shiina, Takeo; Taki, Masao; Shinohara, Naoki; Miyakoshi, Junji

    2016-01-01

    To investigate the cellular effects of terahertz (THz) exposure, human corneal epithelial (HCE-T) cells derived from human eye were exposed to 0.12 THz radiation at 5 mW/cm2 for 24 h, then the genotoxicity, morphological changes, and heat shock protein (Hsp) expression of the cells were examined. There was no statistically significant increase in the micronucleus (MN) frequency of cells exposed to 0.12 THz radiation compared with sham-exposed controls and incubator controls, whereas the MN frequency of cells treated with bleomycin for 1 h (positive control) did increase significantly. Similarly, there were no significant morphological changes in cells exposed to 0.12 THz radiation compared to sham-exposed controls and incubator controls, and Hsp expression (Hsp27, Hsp70, and Hsp90α) was also not significantly different between the three treatments. These results indicate that exposure to 0.12 THz radiation using the present conditions appears to have no or very little effect on MN formation, morphological changes, and Hsp expression in cells derived from human eye. PMID:27527204

  8. Twenty Four-Hour Exposure to a 0.12 THz Electromagnetic Field Does Not Affect the Genotoxicity, Morphological Changes, or Expression of Heat Shock Protein in HCE-T Cells.

    Science.gov (United States)

    Koyama, Shin; Narita, Eijiro; Shimizu, Yoko; Shiina, Takeo; Taki, Masao; Shinohara, Naoki; Miyakoshi, Junji

    2016-08-05

    To investigate the cellular effects of terahertz (THz) exposure, human corneal epithelial (HCE-T) cells derived from human eye were exposed to 0.12 THz radiation at 5 mW/cm² for 24 h, then the genotoxicity, morphological changes, and heat shock protein (Hsp) expression of the cells were examined. There was no statistically significant increase in the micronucleus (MN) frequency of cells exposed to 0.12 THz radiation compared with sham-exposed controls and incubator controls, whereas the MN frequency of cells treated with bleomycin for 1 h (positive control) did increase significantly. Similarly, there were no significant morphological changes in cells exposed to 0.12 THz radiation compared to sham-exposed controls and incubator controls, and Hsp expression (Hsp27, Hsp70, and Hsp90α) was also not significantly different between the three treatments. These results indicate that exposure to 0.12 THz radiation using the present conditions appears to have no or very little effect on MN formation, morphological changes, and Hsp expression in cells derived from human eye.

  9. Effect of physical fitness and endurance exercise on indirect biomarkers of growth hormone and insulin misuse: Immunoassay-based measurement in urine samples.

    Science.gov (United States)

    Pichini, Simona; Ventura, Rosa; Palmi, Ilaria; di Carlo, Simonetta; Bacosi, Antonella; Langohr, Klaus; Abellan, Rosario; Pascual, Jose Antonio; Pacifici, Roberta; Segura, Jordi; Zuccaro, Piergiorgio

    2010-12-01

    Indirect biomarkers of recombinant human growth hormone (rhGH), insulin-like growth factor-I (IGF-I), insulin-like growth factor-II (IGF-II), insulin-like growth factor binding proteins (IGFBP-2 and IGFBP-3) and insulin (C-peptide) were measured together with urinary parameters of renal damage (beta(2)-microglobulin and proteinuria) by immunoassays, in house validated for the purpose, in 61 subjects (36 elite athletes, 18 recreational athletes and 7 sedentary individuals) with different levels of physical fitness and endurance exercise. Validation parameters were good for the evaluated assays, excluding a high inter-assay imprecision and inaccuracy of 24 and 26% obtained for GH assay. The range of concentrations found in urine samples under investigation was generally covered by the calibration curves of the studied immunoassays. However, for the samples below or above the calibration curve, opportune dilution or concentration were performed. Particularly, C-peptide samples had to be diluted 1:5 and beta(2)-microglobulin ones assayed using a triple sample volume, to fall within the calibration range. Urinary C-peptide was the only biomarker statistically higher in samples of elite athletes when compared to recreational athletes and sedentary individuals. Among elite athletes, tae-kwon-do athletes showed the highest IGF-II basal values while weightlifting athletes showed the lower IGF-I and IGFBP-3 basal values. The trend observed in weightlifters' basal samples was confirmed in their training samples: IGF-I, IGF-II, IGFBP-3 and beta(2)-microglobulin were lower in with respect to those from synchronised swimming. Over the training season, within athlete variability was observed for IGFBP-3 for weightlifting athletes. In the studied subjects, no direct associations were found between biomarkers of GH or insulin misuse and urinary parameters of renal damage, eventually due to high-workload endurance training. The variations observed in different biomarkers should be

  10. Preparation of stir cake sorptive extraction based on poly(4-vinylbenzoic acid-divinylbenzene) monolith and its application in sensitive determination of β-agonists in milk and swine urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Xiaojia, E-mail: hxj@xmu.edu.cn; Chen, Linli; Yuan, Dongxing

    2013-11-15

    Highlights: • A new poly(4-vinylbenzoic acid-divinylbenzene) monolith was first prepared. • The porous monolith was used as sorbent of stir cake sorptive extraction. • The new sorbent could extract β-agonists effectively by multiple interactions. • Method of determination of trace β-agonists in milk and urine samples was developed. -- Abstract: In this study, a new stir cake sorptive extraction (SCSE) based on poly(4-vinylbenzoic acid-divinylbenzene) (VBADB) monolith was prepared. The effect of preparation conditions of monolith on extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury intrusion porosimetry and scanning electron microscopy were used to characterize the monolithic material. The combination of SCSE-VBADB with high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) detection was developed for sensitive determination of ultra-trace β-agonists in milk and swine urine samples. In order to obtain the optimal extraction conditions of SCSE-VBADB for β-agonists, several extractive parameters, including pH values and ionic strength in sample matrix, extraction and desorption time were optimized. Under the optimum conditions, the limits of detection (S/N = 3) for the target analytes were 0.007–0.030 μg/L in milk and 0.002–0.011 μg/L in swine urine, respectively. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of both <10.0%, respectively. Finally, the proposed method was successfully used to detect β-agonists in different milk and swine urines samples. Acceptable recoveries ranged from 50.3% to 113% and 50.1% to 92.2% for milk and swine urine samples, respectively; and the RSDs for reproducibility were less than 8.0% for target analytes in all real samples.

  11. A Point-of-Care Immunosensor for Human Chorionic Gonadotropin in Clinical Urine Samples Using a Cuneated Polysilicon Nanogap Lab-on-Chip.

    Directory of Open Access Journals (Sweden)

    S R Balakrishnan

    Full Text Available Human chorionic gonadotropin (hCG, a glycoprotein hormone secreted from the placenta, is a key molecule that indicates pregnancy. Here, we have designed a cost-effective, label-free, in situ point-of-care (POC immunosensor to estimate hCG using a cuneated 25 nm polysilicon nanogap electrode. A tiny chip with the dimensions of 20.5 × 12.5 mm was fabricated using conventional lithography and size expansion techniques. Furthermore, the sensing surface was functionalized by (3-aminopropyltriethoxysilane and quantitatively measured the variations in hCG levels from clinically obtained human urine samples. The dielectric properties of the present sensor are shown with a capacitance above 40 nF for samples from pregnant women; it was lower with samples from non-pregnant women. Furthermore, it has been proven that our sensor has a wide linear range of detection, as a sensitivity of 835.88 μA mIU(-1 ml(-2 cm(-2 was attained, and the detection limit was 0.28 mIU/ml (27.78 pg/ml. The dissociation constant Kd of the specific antigen binding to the anti-hCG was calculated as 2.23 ± 0.66 mIU, and the maximum number of binding sites per antigen was Bmax = 22.54 ± 1.46 mIU. The sensing system shown here, with a narrow nanogap, is suitable for high-throughput POC diagnosis, and a single injection can obtain triplicate data or parallel analyses of different targets.

  12. A Point-of-Care Immunosensor for Human Chorionic Gonadotropin in Clinical Urine Samples Using a Cuneated Polysilicon Nanogap Lab-on-Chip.

    Science.gov (United States)

    Balakrishnan, S R; Hashim, U; Gopinath, Subash C B; Poopalan, P; Ramayya, H R; Iqbal Omar, M; Haarindraprasad, R; Veeradasan, P

    2015-01-01

    Human chorionic gonadotropin (hCG), a glycoprotein hormone secreted from the placenta, is a key molecule that indicates pregnancy. Here, we have designed a cost-effective, label-free, in situ point-of-care (POC) immunosensor to estimate hCG using a cuneated 25 nm polysilicon nanogap electrode. A tiny chip with the dimensions of 20.5 × 12.5 mm was fabricated using conventional lithography and size expansion techniques. Furthermore, the sensing surface was functionalized by (3-aminopropyl)triethoxysilane and quantitatively measured the variations in hCG levels from clinically obtained human urine samples. The dielectric properties of the present sensor are shown with a capacitance above 40 nF for samples from pregnant women; it was lower with samples from non-pregnant women. Furthermore, it has been proven that our sensor has a wide linear range of detection, as a sensitivity of 835.88 μA mIU(-1) ml(-2) cm(-2) was attained, and the detection limit was 0.28 mIU/ml (27.78 pg/ml). The dissociation constant Kd of the specific antigen binding to the anti-hCG was calculated as 2.23 ± 0.66 mIU, and the maximum number of binding sites per antigen was Bmax = 22.54 ± 1.46 mIU. The sensing system shown here, with a narrow nanogap, is suitable for high-throughput POC diagnosis, and a single injection can obtain triplicate data or parallel analyses of different targets.

  13. 大深度饱和潜水对潜水员尿量及尿中微量元素的影响%Effects of deep saturation diving on urine volume and trace elements in the urine of the divers

    Institute of Scientific and Technical Information of China (English)

    柯晓安; 高鉴; 王燎原; 赵于瑜

    2015-01-01

    Objective To observe the effects of deep saturation diving on urine volume and trace elements in the urine of the divers , so as to provide theoretical evidence for medical support of deep saturation diving operations and health promotion of divers .Methods Four male healthy divers participated in the 480 msw simulated saturation dive .Twenty-four-hour urine samples were collected the day before entrance into the chamber , during their stay daily in the chamber , and the day after they came out of the chamber .The contents of Ba, Co, Cr, Cu, Fe, Mn, Pb, Sr, Zn in the urine samples were determinated with inductively coupled plasma atomic emission spectrometry , and the data obtained were analyzed with LSD variance analysis .Results Urine volumes of the divers at days 4, 7, 8, 10, 17 and 18 in the chamber were significantly higher than those of both day 1 before enterance into the chamber and the day after surfacing out of the chamber .The urine volume at day 15 in the chamber was significantly higher than that of 1 day before enterance into the chamber . In the 24 h urine samples, the excretion of Ba reached peak at days 10 and 11, and urine volumes at days 16, 18, 19 were significantly lower than those at days 1-11.The excretions of Cr and Co at days 16, 18 and 19 were significantly lower than those at days 1-11.The peak excretions of Fe and Mn all appeared at days 10 and 11, and the peak excretion of Pb was at days 8 and 10.However, the peak excretion of Sr was relatively stable, reaching the peak at day 12.The peak excretion of Zn was at day 8, then decreased gradually and finally reached the bottom at day 19.The peak excretion of Cu at day 10 increased sharply , then decreased gradually and reached bottom at day 19.Conclusions Deep saturation diving exerted certain effects on the urine volume and the metabolism of trace elements in urine in divers .Further research efforts should be made in this respect, so as to provide better medical support and promote the

  14. Codetection of Trichomonas vaginalis and Candida albicans by PCR in Urine Samples in a Low-Risk Population Attended in a Clinic First Level in Central Veracruz, Mexico

    Directory of Open Access Journals (Sweden)

    A. López-Monteon

    2013-01-01

    Full Text Available The aim of this study is to estimate the prevalence of Trichomonas vaginalis and Candida albicans in low-risk patients treated at a first level clinic (primary health care represents the first level of contact of individuals, families, and the community with the system national health. Using a cross-sectional study in patients treated in clinical laboratory of the Sanitary District no. 7 of the city of Orizaba during the months June-July, 252 urine samples were collected for the identification of T. vaginalis and C. albicans by PCR. Furthermore, we analyzed the sociodemographic characteristics of the studied population. We observed an overall prevalence of 23.41% (95% CI 22.10–24.72 for T. vaginalis and 38.88% (95% CI 37.73–40.03 for C. albicans. There was also presence of coinfection in 14.28% (95% CI 13.10–15.46, which was associated with the presence of pain. Most of the positive cases were observed in women house-maker (80%, 95% CI 50.36–48.98. The results of this study provide evidence that the majority of positive cases observed in the studied population are presented in an asymptomatic form and usually are not associated with any risk factor.

  15. Ultrasound assisted combined molecularly imprinted polymer for selective extraction of nicotinamide in human urine and milk samples: Spectrophotometric determination and optimization study.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

    2017-01-01

    Ultrasound-assisted dispersive solid phase microextraction followed by UV-vis spectrophotometer (UA-DSPME-UV-vis) was designed for extraction and preconcentration of nicotinamide (vitamin B3) by HKUST-1 metal organic framework (MOF) based molecularly imprinted polymer (MIP). This new material was characterized by FTIR and FE-SEM techniques. The preliminary Plackett-Burman design was used for screening and subsequently the central composite design justifies significant terms and possible construction of mathematical equation which give the individual and cooperative contribution of variables like HKUST-1-MOF-NA-MIP mass, sonication time, temperature, eluent volume, pH and vortex time. Accordingly the optimum condition was set as: 2.0mg HKUST-1-MOF-NA-MIP, 200μL eluent and 5.0min sonication time in center points other variables were determined as the best conditions to reach the maximum recovery of the analyte. The UA-DSPME-UV-vis method performances like excellent linearity (LR), limits of detection (LOD), limits of quantification of 10-5000μgL(-1) with R(2) of 0.99, LOD (1.96ngmL(-1)), LOQ (6.53μgL(-1)), respectively show successful and accurate applicability of the present method for monitoring analytes with within- and between-day precision of 0.96-3.38%. The average absolute recoveries of the nicotinamide extracted from the urine, milk and water samples were 95.85-101.27%.

  16. Implementation of gradients of organic solvent in micellar liquid chromatography using DryLab(®): separation of basic compounds in urine samples.

    Science.gov (United States)

    Rodenas-Montano, J; Ortiz-Bolsico, C; Ruiz-Angel, M J; García-Alvarez-Coque, M C

    2014-05-30

    In micellar liquid chromatography (MLC), chromatographic peaks are more evenly distributed compared to conventional reversed-phase liquid chromatography (RPLC). This is the reason that most procedures are implemented using isocratic elution. However, gradient elution may be still useful in MLC to analyse mixtures of compounds within a wide range of polarities, decreasing the analysis time. Also, it benefits the determination of moderately to low polar compounds in physiological fluids performing direct injection: an initial micellar eluent with a low organic solvent content, or a pure micellar (without surfactant) solution, will provide better protection of the column against the proteins in the physiological fluid, and once the proteins are swept away, the elution strength can be increased using a positive linear gradient of organic solvent to reduce the analysis time. This work aims to encourage analysts to implement gradients of organic solvent in MLC, which is rather simple and allows rapid analytical procedures without pre-treatment or the need of re-equilibration. The implementation of gradient elution is illustrated through the separation of eight basic compounds (β-blockers) in urine samples directly injected into the chromatograph, the most hydrophobic showing large retention in both conventional RPLC and MLC. The use of the DryLab(®) software to optimise gradients of organic solvent with eluents containing a fixed amount of surfactant above the critical micellar concentration is shown to provide satisfactory predictions, and can facilitate greatly the implementation of gradient protocols.

  17. 高脂血症性胰腺炎患者尿样的代谢组学%Metabonomics study of urine samples of patients with hyperlipidemic pancreatitis

    Institute of Scientific and Technical Information of China (English)

    赵严; 吴建兵; 潘立; 张小雷; 邱云平; 苏明明; 贾伟; 王兴鹏

    2009-01-01

    目的 基于气相色谱质谱的代谢组学分析方法,研究高脂血症性胰腺炎(HLP)患者尿样.通过对其尿样代谢物组的分析和生物标记物的发现,寻找HLP的代谢变化,探讨代谢组学在急性胰腺炎(AP)中的应用.方法 取24例HLP患者尿样及40例年龄、性别匹配的正常健康人尿样,样品经预处理、衍牛和气相色谱质谱分析后,利用正交偏最小方差判别分析(OPISA-DA)的方法,观察健康组和HLP组的代谢轮廓差异.结果 上述方法能清晰地将HLP患者和健康人样本分开,通过NIST、Wiley等谱库搜索分析了21个代谢物(可信度>700).其中用标准品鉴定之后,发现与健康组比较HLP患者尿样中烟酸、乌头酸、柠檬酸、马尿酸、对一羟基苯乙酸、对-羟基苯丙酸含量下降;色氨酸、酪氨酸、酪胺、棕榈油脂、硬脂酸等物质含量上升.代谢组学研究显示HLP患者三羧酸循环、肠道菌群结构、脂肪代谢及氨基酸代谢等发生改变.结论 HLP患者和正常人尿样代谢谱之间存在差异,而且可能从代谢组学分析中找出特异的标志性代谢产物,阐释该疾病的代谢变化;表明利用代谢组学研究尿液中的代谢物,可以为HLP的诊断和发病机制提供一个可借鉴的手段;代谢组学分析是一种有良好发展前景的研究方法.%Objective Metabonomics method based gas chromatography-mass spectrometry (GC/MS)were used to analyze the urine samples of patients with hyperlipidemic pancreatitis (HLP) to describe the characteristics of metabolism changes of HLP,identify potential biomarkers,and investigate the role of metabonomics study in the management of AP.Methods 24 patients of HLP and 40 age,sex matched volunteers were enrolled and their urine samples were collected.The urine samples underwent preparation,derivation and GC/MS analysis,Orthogonal-Projection to Latent Structures-Discriminant Analysis (OPLS-DA)were performed to detect the metabolic profile

  18. Codetection of Trichomonas vaginalis and Candida albicans by PCR in urine samples in a low-risk population attended in a clinic first level in central Veracruz, Mexico.

    Science.gov (United States)

    López-Monteon, A; Gómez-Figueroa, F S; Ramos-Poceros, G; Guzmán-Gómez, D; Ramos-Ligonio, A

    2013-01-01

    The aim of this study is to estimate the prevalence of Trichomonas vaginalis and Candida albicans in low-risk patients treated at a first level clinic (primary health care represents the first level of contact of individuals, families, and the community with the system national health). Using a cross-sectional study in patients treated in clinical laboratory of the Sanitary District no. 7 of the city of Orizaba during the months June-July, 252 urine samples were collected for the identification of T. vaginalis and C. albicans by PCR. Furthermore, we analyzed the sociodemographic characteristics of the studied population. We observed an overall prevalence of 23.41% (95% CI 22.10-24.72) for T. vaginalis and 38.88% (95% CI 37.73-40.03) for C. albicans. There was also presence of coinfection in 14.28% (95% CI 13.10-15.46), which was associated with the presence of pain. Most of the positive cases were observed in women house-maker (80%, 95% CI 50.36-48.98). The results of this study provide evidence that the majority of positive cases observed in the studied population are presented in an asymptomatic form and usually are not associated with any risk factor.

  19. The human urine metabolome.

    Directory of Open Access Journals (Sweden)

    Souhaila Bouatra

    Full Text Available Urine has long been a "favored" biofluid among metabolomics researchers. It is sterile, easy-to-obtain in large volumes, largely free from interfering proteins or lipids and chemically complex. However, this chemical complexity has also made urine a particularly difficult substrate to fully understand. As a biological waste material, urine typically contains metabolic breakdown products from a wide range of foods, drinks, drugs, environmental contaminants, endogenous waste metabolites and bacterial by-products. Many of these compounds are poorly characterized and poorly understood. In an effort to improve our understanding of this biofluid we have undertaken a comprehensive, quantitative, metabolome-wide characterization of human urine. This involved both computer-aided literature mining and comprehensive, quantitative experimental assessment/validation. The experimental portion employed NMR spectroscopy, gas chromatography mass spectrometry (GC-MS, direct flow injection mass spectrometry (DFI/LC-MS/MS, inductively coupled plasma mass spectrometry (ICP-MS and high performance liquid chromatography (HPLC experiments performed on multiple human urine samples. This multi-platform metabolomic analysis allowed us to identify 445 and quantify 378 unique urine metabolites or metabolite species. The different analytical platforms were able to identify (quantify a total of: 209 (209 by NMR, 179 (85 by GC-MS, 127 (127 by DFI/LC-MS/MS, 40 (40 by ICP-MS and 10 (10 by HPLC. Our use of multiple metabolomics platforms and technologies allowed us to identify several previously unknown urine metabolites and to substantially enhance the level of metabolome coverage. It also allowed us to critically assess the relative strengths and weaknesses of different platforms or technologies. The literature review led to the identification and annotation of another 2206 urinary compounds and was used to help guide the subsequent experimental studies. An online database

  20. Simultaneous determination of N-hydroxymethyl-N-methylformamide, N-methylformamide and N-acetyl-S-(N-methylcarbamoyl)cystein in urine samples from workers exposed to N,N-dimethylformamide by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Sohn, Jae Ho; Han, Min Jeong; Lee, Mi Young; Kang, Seong-Kyu; Yang, Jeong Sun

    2005-02-07

    N-Hydroxymethyl-N-methylformamide (HMMF) and N-methylformamide (NMF) in urine samples from workers exposed to N,N-dimethylformamide (DMF) cannot be distinguished by a gas chromatographic method because HMMF is converted to NMF at the injection port of gas chromatography (GC). Total NMF (HMMF+NMF) has been measured instead. Also, the determination of N-acetyl-S-(N-methylcarbamoyl)cystein (AMCC), which is supposed to be related to the toxicity of DMF, needs multiple treatments to convert to a volatile compound before GC analysis. There is no previous report of a simultaneous determination of three major metabolites of DMF in urine. The aim of this study is to develop a simple and selective method for the determination of DMF metabolite in urine. By using a liquid chromatography-tandem mass spectrometry, we can directly distinguish these three major metabolites of DMF in a single run. The diluted urine samples were analyzed on Capcell Pak MF SG80 column with the mobile phase of methanol in 2mM formic acid (10:90, v/v). The analytes were detected by an electrospray ionization tandem mass spectrometry in the multiple-reaction-monitoring mode. The standard curves were linear (r>0.999) over the concentration ranges of 0.004-8 microg/mL. The precision and accuracy of quality control samples for inter-batch (n=6) analyses were in the range of 1.3-9.8% and 94.7-116.8, respectively. The sum of each HMMF and NMF concentration determined by LC-MS/MS method shows high correlation (r=0.9927 with the slope of 1.0415, p<0.0001) with NMF included HMMF concentration determined by GC method for 13 urine samples taken from workers exposed to DMF. The excretion ratio of HMMF:NMF:AMCC is approximately 4:1:1 in molar concentration.

  1. Screening for human papillomavirus: Is urine useful?

    Directory of Open Access Journals (Sweden)

    K W D′Hauwers

    2009-01-01

    We looked at the usefulness of urine as a tool for HPV screening. Pubmed was searched with the words ′′HPV′′, ′′Urine,′′ and ′′HPV-DNA′′. The chance of finding HPV-DNA in urine is higher in men with lesions in the urethra than outside the urethra, and in women with abnormal cervical cytology. In general, the results of testing urine for HPV-DNA are better for women than for men, probably because of the anatomical position of the urethra to the vagina, vulva, and cervix. In both genders, urine HPV prevalence is higher in HIV pos patients and in high-risk populations. Urine, to screen asymptomatic low-risk-profile (women seems less useful because their urine samples are often inadequate. If urine proves to be the best medium to screen, a low-risk population remains controversial.

  2. Pharmacokinetics of dilevalol and its conjugates in man. Assay method for plasma, blood, urine and bile samples and preliminary pharmacokinetic studies.

    Science.gov (United States)

    Neubeck, M; Becker, C; Henke, D; Rösch, W; Spahn-Langguth, H; Mutschler, E

    1993-09-01

    The renal and biliary excretion of the beta-adrenoceptor blocking agent dilevalol (CAS 75659-07-3) and its conjugates was examined in a preliminary pharmacokinetic study. Plasma, urine and bile dilevalol concentrations were determined with a simplified procedure that is based on alkaline liquid-liquid extraction using diethyl ether and subsequent reversed-phase HPLC separation of the reconstituted samples (on a PRP-1 stationary phase using a mixture of methanol and pH 9.8 carbonate buffer as mobile phase). Triamterene was used as internal standard. The quantification of the conjugates was accomplished indirectly via enzymatic hydrolysis (glusulase) with and without addition of the beta-glucuronidase inhibitor 1,4-saccharolactone (at a final concentration of 5.5 mmol/l). In the pharmacokinetic study healthy volunteers and cholecystectomised patients with a T-drain received a single oral dose of 200 mg dilevalol. Furthermore, to healthy volunteers an i.v. dose of 60 mg dilevalol was given in order to estimate the absolute bioavailability. From the obtained data the systemic plasma clearance was calculated to be 1708 ml/min. The oral bioavailability was calculated to be 16%. The log concentration-time curves of the metabolites paralleled those of dilevalol in the terminal section with average terminal half-lives of approx. 5 h. In volunteers the fractions of the dose excreted renally were 0.5% for parent drug, 23% for the glucuronide(s) and 8% for the sulfate. The corresponding values found for the patients were not significantly different. In the patients' bile only 1.2% of the total dose were found (0.03% dilevalol, 1.1% dilevalol glucuronide(s), 0.1% dilevalol sulfate).(ABSTRACT TRUNCATED AT 250 WORDS)

  3. Mass spectrometric studies on the in vivo metabolism and excretion of SIRT1 activating drugs in rat urine, dried blood spots, and plasma samples for doping control purposes.

    Science.gov (United States)

    Höppner, Sebastian; Delahaut, Philippe; Schänzer, Wilhelm; Thevis, Mario

    2014-01-01

    The NAD(+) depending enzyme SIRT1 regulates the mitochondrial biogenesis, fat and glucose metabolism through catalyzing the deacetylation of several metabolism-related protein-substrates. Recently, synthetic activators of SIRT1 referred to as STACs (Sirtuin activating compounds, e.g. SRT2104) were identified and tested in clinical studies for the treatment of aging-related diseases such as type 2 diabetes, Alzheimer's and obesity. Although the mechanism of SIRT1 activation by small molecules has caused considerable controversy, STACs demonstrated a significant performance enhancement in mice experiments including an improvement of endurance, muscle strength, and locomotor behavior. Due to their potential to increase exercise tolerance in healthy individuals, SIRT1 activators are currently being monitored by anti-doping authorities. In the present study, the in vivo metabolic clearance of three SIRT1 activators was investigated in rats by the collection of urine, DBS (dried blood spots) and plasma samples following a single oral administration. The resulting metabolic products were studied by positive electrospray ionization - (tandem) mass spectrometry and confirmed by the comparison with in vitro generated metabolites using human and rat liver microsomal preparations. Subsequently, a screening procedure for five SIRT1 activators and the metabolite M1-SRT1720 in DBS specimens was developed. Liquid-liquid-extraction and liquid chromatography/tandem mass spectrometry was employed based on diagnostic ion transitions recorded in multiple reaction monitoring mode and two deuterated internal standards namely d8-SRT1720 and d8-M1-SRT1720 were utilized. The doping control assay was characterized with regard to specificity, limit of detection (10-50ng/ml), recovery (65-83%) and imprecision (7-20%) and ion suppression/enhancement effects (sports drug testing applications.

  4. 尿液标本淋球菌多抗原序列分型研究%Neisseria gonorrhoeae multi-antigen sequence typing using urine samples

    Institute of Scientific and Technical Information of China (English)

    陈绍椿; 尹跃平; 施美琴; 戴秀芹; 韩燕; 王宝玺; 陈祥生

    2013-01-01

    province,Jiangmen and Maoming cities of Guangdong province.Methods DNA was extracted using Qiagen DX extraction kits from 88 urine samples which were collected from male patients attending sexually transmitted disease (STD) clinics and positive for nucleic acid amplification test (NAAT) for N.gonorrhoeae.Two rounds of PCR were carried out to amplify the porB and tbpB genes of N.gonorrhoeae followed by gene sequencing.Sequence alignment was performed on the NG-MAST website (http://www.ng-mast.net) to determine the genotype of N.gonorrhoeae.Results The first-round PCR yielded positive results for porB and tbpB in 13.6% (12/88) and 14.8% (13/88),respectively,of these urine specimens,and 12 samples were successfully genotyped with the efficiency of genotyping being 13.6%.The amplification efficiency of second-round PCR was enhanced to 71.6% and 72.7% for porB and tbpB,respectively,and the efficiency of genotyping increased to 70.5% (62/88).Compared with the first-round PCR,the second-round PCR showed an increase in amplification efficiency for porB and tbpB by 58.0% and 57.9% respectively,as well as in genotyping efficiency by 56.9%.Forty-five genotypes were identified in the 62 samples,including 40 known genotypes and 5 novel genotypes.Of these genotypes,ST1866 was the most abundant (6/62),followed by ST1972 (4/62) and ST3356 (4/62),all of which were from Jiangsu province.The ST532 genotype was identified in 3 samples from Guangdong province,ST2221 genotype in 2 samples from Guangxi Zhuang Autonomous region.Each of the remaining genotypes was identified in only 1 sample and scattered in all of these cities.The 5 novel MAST-genotypes were as follows:porB-892 and tbpB-46 (98% similarity),porB-130 and tbpB-504 (96% similarity),porB-2790 and tbpB-32 (99% similarity),porB-1053 and tbpB-856 (99% similarity).Conclusions Urine samples can be used for NG-MAST analysis,and two rounds of PCR can enhance the efficiency of genotyping.NG-MAST genotypes appear to

  5. Urine - abnormal color

    Science.gov (United States)

    ... medlineplus.gov/ency/article/003139.htm Urine - abnormal color To use the sharing features on this page, please enable JavaScript. The usual color of urine is straw-yellow. Abnormally colored urine ...

  6. [Bacterial contamination of infant urine samples obtained from filter papers used in neuroblastoma-screening tests. (6) Protective effects of preaddition of chlorhexidine digluconate in filter papers or containers for urine on bacterial break-down of creatinine, vanillylmandelic acid and homovanillic acid].

    Science.gov (United States)

    Imai, J; Iwata, H; Gotoh, K; Mori, H; Kawai, M

    1992-10-01

    The effects of chlorhexidine digluconate preadded to urine samples for a neuroblastoma-screening test in preventing the break-down of creatinine (Cre), vanillylmandelic acid (VMA), and homovanillic acid (HVA) by creatinine-cleaving bacteria and the influence of the added disinfectant on the HPLC determination of urinary Cre, VMA, vanillillactic acid (VLA) and HVA. Laboratory or field experiments showed that preadded disinfectant (0.02% volume) nearly completely inhibited the growth of the bacteria and satisfactorily protected urinary Cre, VMA, and HVA from bacterial decomposition. Chlorhexidine digluconate was comparable to benzalkonium chloride in its inhibitory effects on the growth and activities of creatinine-cleaving bacteria. Unlike benzalkonium chloride, chlorhexidine digluconate added to urine samples gave no troubles in subsequent analytical processes. Addition of the disinfectant (0.02% volume) to standard Cre, VMA, VLA, and HVA solution did not affect retention times and sensitivities in HPLC analyses. To estimate influences of the added disinfectant on the serial HPLC determinations of VMA, VLA, and HVA on a large number of urine samples (40, 80, 120, 160, 200, or 5, 500), HPLC analyses were performed on standard VMA, VLA, and HVA solution with repeated injection of the disinfectant in great amounts into a column. The results showed no appreciable changes in the retention times and sensitivities of VMA, VLA, and HVA, and almost complete elution of the disinfectant retained on the column were possible with water-methanol (1:1, 2:8) or methanol washing.(ABSTRACT TRUNCATED AT 250 WORDS)

  7. Preparation of water stable methyl-modified metal-organic framework-5/polyacrylonitrile composite nanofibers via electrospinning and their application for solid-phase extraction of two estrogenic drugs in urine samples.

    Science.gov (United States)

    Asiabi, Mina; Mehdinia, Ali; Jabbari, Ali

    2015-12-24

    The nanofibers of methyl-modified metal-organic framework-5/polyacrylonitrile composite (CH3MOF-5/PAN) were successfully synthesized and used as a solid-phase extraction (SPE) sorbent for pre-concentration of two estrogenic drugs, levonorgestrel and megestrol acetate, in urine samples. A simple, cheap and accessible electrospinning method was employed to prepare a water stable CH3MOF-5/PAN composite. The nanofibers were packed into the mini-disc cartridges to be used as SPE devices. They were also characterized by scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, X-ray diffraction and N2 adsorption-desorption experiments. The effects of different parameters influencing the extraction efficiency including the type of eluent and its volume, the amount of the sorbent, pH, the ionic strength, the sample volume and the reusability of the sorbent were investigated and optimized. Under the optimized conditions, the linearity varied in range of 0.05-100μgL(-1) with R(2) values higher than 0.999. The limit of detection for both of the analytes was 0.02μgL(-1). The applicability of the method was examined by analyzing the analytes in the urine samples. The recovery of the analytes varied in the range of 82.8-94.8% which shows capability of the method for the determination of the drugs in the urine samples.

  8. Hollow fibre-supported liquid membrane extraction and LC-MS/MS detection for the analysis of heterocyclic amines in urine samples

    DEFF Research Database (Denmark)

    Busquets, R.; Jonsson, J. A.; Frandsen, Henrik Lauritz

    2009-01-01

    . The analytical method consisted of extraction and clean-Lip by the novel technique liquid-phase microextraction combined with LC-MS/MS. The effect of pH during the extraction and hydrolysis step was examined. High sensitivity was achieved when the extraction was performed in raw urine adjusted to pH 5.5, 2-amino...

  9. Simultaneous determination of hydroxycinnamates and catechins in human urine samples by column switching liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry

    DEFF Research Database (Denmark)

    Nielsen, Salka E.; Sandström, B.

    2003-01-01

    by atmospheric pressure chemical ionization (APCI) MS using single ion monitoring (SIM) in negative mode. Linear calibration graphs were achieved in the dynamic range of 10-1000 ng/ml urine. The inter- and intraassay coefficients of variation (C.V.%) for the analysis of the four compounds in quality control...

  10. Urine Protein and Urine Protein to Creatinine Ratio

    Science.gov (United States)

    ... products and services. Advertising & Sponsorship: Policy | Opportunities Urine Protein and Urine Protein to Creatinine Ratio Share this page: Was this page helpful? Also known as: 24-Hour Urine Protein; Urine Total Protein; Urine Protein to Creatinine Ratio; ...

  11. Quantitative determination of 8-isoprostaglandin F(2α) in human urine using microfluidic chip-based nano-liquid chromatography with on-chip sample enrichment and tandem mass spectrometry.

    Science.gov (United States)

    Bai, Hsin-Yu; Lin, Shu-Ling; Chung, Yu-Ting; Liu, Tsung-Yun; Chan, Shan-An; Fuh, Ming-Ren

    2011-04-15

    Urinary 8-isoprostaglandin F(2α) (8-isoPGF(2α)) has been reported as an important biomarker to indicate the oxidative stress status in vivo. In order to quantitatively determine the low contents of 8-isoPGF(2α) (in sub- to low ng mL(-1) range) in physiological fluids, a sensitive detection method has become an important issue. In this study, we employed a microfluidic chip-based nano liquid chromatography (chip-nanoLC) with on-chip sample enrichment coupled to triple quadrupole mass spectrometer (QqQ-MS) for the quantitative determination of 8-isoPGF(2α) in human urine. This chip-nanoLC unit integrates a microfluidic switch, a chip column design having a pre-column (enrichment column) for sample enrichment prior to an analytical column for separation, as well as a nanospray emitter on a single polyimide chip. The introduction of enrichment column offers the advantages of online sample pre-concentration and reducing matrix influence on MS detection to improve sensitivity. In this study, the chip-nanoLC consisting of Zorbax 300A SB-C18 columns and Agilent QqQ Mass spectrometer were used for determining 8-isoPGF(2α) in human urine. Gradient elution was employed for effective LC separation and multiple reaction monitoring (MRM) was utilized for the quantitative determination of 8-isoPGF(2α) (m/z 353→193). We employed liquid-liquid extraction (LLE)/solid-phase extraction (SPE) for extracting analyte and reducing matrix effect from urine sample prior to chip-nanoLC/QqQ-MS analysis for determining urinary 8-isoPGF(2α). Good recoveries were found to be in the range of 83.0-85.3%. The linear range was 0.01-2 ng mL(-1) for urinary 8-isoPGF(2α). In addition, the proposed method showed good precision and accuracy for 8-isoPGF(2α) spiked synthetic urine samples. Intra-day and inter-day precisions were 1.8-5.0% and 4.3-5.8%, respectively. The method accuracy for intra-day and inter-day assays ranged from 99.3 to 99.9% and 99.4 to 99.7%, respectively. Due to its

  12. Determination of Amphetamine, Amfepramone and Fenproporex in Urine Samples by HPLC-DAD: Application to a Population of Brazilian Truck Drivers

    OpenAIRE

    Takitane,Juliana; Almeida, Rafael M.; Tiago F. de Oliveira; Prado,Natanael V.; Muñoz,Daniel R.; Leyton,Vilma; Yonamine, Mauricio

    2016-01-01

    Commercially available immunoassay tests are designed to detect the presence of amphetamine/methamphetamine or methylenodioxyamphetamines. However, it is known that Brazilian truck drivers also report the use of other illicit amphetamines, such as amfepramone and fenproporex. Thus, a method was developed and validated in order to quantify amphetamine-type stimulants (amphetamine, fenproporex and amfepramone) in urine by high performance liquid chromatography with diode array detection (HPLC-D...

  13. Simultaneous derivatization and solid-based disperser liquid-liquid microextraction for extraction and preconcentration of some antidepressants and an antiarrhythmic agent in urine and plasma samples followed by GC-FID.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Khorram, Parisa; Ghorbanpour, Houshang

    2015-03-01

    The present work is based on a one-step method including derivatization and solid-based disperser liquid-liquid microextraction followed by gas chromatography-flame ionization detection (GC-FID) for the determination of four antidepressants (fluoxetine, fluvoxamine, tranylcypromine, and nortriptyline) and an antiarrhythmic agent (mexiletine) in human urine and plasma samples. In this method, a mixture of 1,1,2,2-tetrachloroethane (extraction solvent) and butylchloroformate (derivatizing reagent) is added on a sugar cube (solid disperser) and it is introduced into an aqueous sample containing the analytes and a catalyst, e.g. 3-methylpyridine (picoline). During dissolving the sugar cube by manual shaking, the extractant and derivatization agent are gradually released into the sample as very fine droplets. Then the resulted cloudy solution is centrifuged and the sedimented phase is analyzed by GC-FID. The influence of several variables on the efficiency of derivatization/microextraction procedure such as kind and volume of extraction solvent, type and amount of disperser, amount of derivatization agent, and catalyst volume are optimized. Under the optimum conditions the calibration curves are linear in the range of 8-100,000μgL(-1) (coefficient of determination ≥0.994). The relative standard deviations are obtained in the range of 3.0-6.0% for all compounds. Moreover, the detection limits and enrichment factors of the target analytes are obtained in the ranges 1-15μgL(-1) and 228-268, respectively, for both plasma and urine samples. The relative recoveries obtained for the spiked plasma and urine samples are between 70 and 91%. The results show that the proposed method is simple, reliable, low cost, and applicable to determine trace amounts of the studied drugs in biological samples.

  14. High-throughput sample preparation for the quantitation of acephate, methamidophos, omethoate, dimethoate, ethylenethiourea, and propylenethiourea in human urine using 96-well-plate automated extraction and high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Jayatilaka, Nayana K; Angela Montesano, M; Whitehead, Ralph D; Schloth, Sara J; Needham, Larry L; Barr, Dana Boyd

    2011-07-01

    Acephate, methamidophos, o-methoate, and dimethoate are organophosphorus pesticides, and ethylenethiouria and propylenethiourea are two metabolites from the bisdithiocarbamate fungicide family. They are some of the most widely used pesticides and fungicides in agriculture both domestically and abroad. The existing high-performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) method for the measurement of these compounds in human urine was improved by using a 96-well plate format sample preparation; the use of HPLC-MS/MS was comparable with a concentration range of 0.125 to 50 ng/ml. Deuterium-labeled acephate, ethylenethiouria, and methamidophos were used as internal standards. The sample preparation procedure, in the 96-well format with a 0.8-ml urine sample size, uses lyophilization of samples, followed by extraction with dichloromethane. The analytes were chromatographed on a Zorbax SB-C3 (4.6 × 150 mm, 5.0-μm) column with gradient elution by using 0.1% formic acid in aqueous solution (solvent A) and 0.1% formic acid in methanol (solvent B) mobile phase at a flow rate of 1 ml/min. Quantitative analysis was performed by atmospheric pressure chemical ionization source in positive ion mode using multiple-reaction monitoring of the precursor-to-product ion pairs for the analytes on a TSQ Quantum Ultra HPLC-MS/MS. Repeated analyses of urine samples spiked with high (15 ng/ml), medium (5 ng/ml), and low (1 ng/ml) concentrations of the analytes gave relative SDs of <13%. The limits of detection were in the range of 0.004-0.01 ng/ml. The method also has high accuracy, high precision, and excellent extraction recovery. Furthermore, the improved sample preparation method decreased the cost and labor required while effectively doubling the analytic throughput with minimal matrix effect.

  15. Classical Molecular Tests Using Urine Samples as a Potential Screening Tool for Human Papillomavirus Detection in Human Immunodeficiency Virus-Infected Women

    OpenAIRE

    Munoz, Marina; Camargo, Milena; Soto-De Leon, Sara C.; Sanchez, Ricardo; Pineda-Peña, Andrea C.; Perez-Prados, Antonio; Patarroyo, Manuel E.; Patarroyo, Manuel A.

    2013-01-01

    Human papillomavirus (HPV) is the main risk factor associated with the development of cervical cancer (CC); however, there are other factors, such as immunosuppression caused by the human immunodeficiency virus (HIV), that favor progression of the illness. This study was thus aimed at evaluating the functionality of classical PCR-based molecular tests for the generic identification of HPV DNA (GP5+/GP6+, MY09/MY11, and pU1M/2R primers, individually or in combination) using cervical and urine ...

  16. A fast method for bisphenol A and six analogues (S, F, Z, P, AF, AP) determination in urine samples based on dispersive liquid-liquid microextraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Rocha, Bruno Alves; da Costa, Bruno Ruiz Brandão; de Albuquerque, Nayara Cristina Perez; de Oliveira, Anderson Rodrigo Moraes; Souza, Juliana Maria Oliveira; Al-Tameemi, Maha; Campiglia, Andres Dobal; Barbosa, Fernando

    2016-07-01

    In this study, a novel method combining dispersive liquid-liquid microextraction (DLLME) and fast liquid chromatography coupled to mass spectrometry (LC-MS/MS) was developed and validated for the extraction and determination of bisphenol A (BPA) and six bisphenol analogues, namely bisphenol S (BPS), bisphenol F (BPF), bisphenol P (BPP), bisphenol Z (BPZ), bisphenol AP (BPAP) and bisphenol AF (BPAF) in human urine samples. Type and volume of extraction and disperser solvents, pH sample, ionic strength, and agitation were evaluated. The matrix-matched calibration curves of all analytes were linear with correlation coefficients higher than 0.99 in the range level of 0.5-20.0ngmL(-1). The relative standard deviation (RSD), precision, at three concentrations (1.0, 8.0 and 15.0ngmL(-1)) was lower than 15% with accuracy ranging from 90 to 112%. The biomonitoring capability of the new method was confirmed with the analysis of 50 human urine samples randomly collected from Brazilians. BPA was detected in 92% of the analyzed samples at concentrations ranging

  17. Improvement in quantification of urine components: Alternate technique

    CERN Document Server

    Kumar, S

    2014-01-01

    Urea and creatinine are two important diagnostic components of urine. The study of creatinine in liquid phase is difficult due to its feeble concentration in urine. To bring down the detection limit, DCD Raman spectroscopy was employed. Raman studies in association with partial least square algorithm of artificial urine samples gave improved results in dried phase as compared to liquid phase. These findings were further validated on real urine samples.

  18. Urine specific gravity test

    Science.gov (United States)

    ... medlineplus.gov/ency/article/003587.htm Urine specific gravity test To use the sharing features on this page, please enable JavaScript. Urine specific gravity is a laboratory test that shows the concentration ...

  19. Protein urine test

    Science.gov (United States)

    ... Urine albumin; Proteinuria; Albuminuria Images White nail syndrome Protein urine test References Gerber GS, Brendler CB. Evaluation of the urologic patient: history, physical examination, and urinalysis. In: Wein AJ, Kavoussi ...

  20. Urine drug screen

    Science.gov (United States)

    Drug screen -- urine ... detect the presence of illegal and some prescription drugs in your urine. Their presence indicates that you recently used these drugs. Some drugs may remain in your system for ...

  1. Urine concentration test

    Science.gov (United States)

    ... page: //medlineplus.gov/ency/article/003608.htm Urine concentration test To use the sharing features on this page, please enable JavaScript. A urine concentration test measures the ability of the kidneys to ...

  2. Magnetic Solid-Phase Extraction Using Fe3O4@SiO2 Magnetic Nanoparticles Followed by UV-Vis Spectrometry for Determination of Paraquat in Plasma and Urine Samples

    OpenAIRE

    Ou Sha; Yu Wang; Xin Yin; Xiaobing Chen; Li Chen; Shujun Wang

    2017-01-01

    A rapid and simple method was optimized and validated for the separation and quantification of paraquat, a frequently used herbicide and a leading cause of fatal poisoning worldwide, at trace levels with UV-Vis spectrophotometry in plasma and urine samples by direct magnetic solid-phase extraction. Fe3O4@SiO2 nanoparticles (NPs) were used as the magnetic solid-phase extraction agents and the paraquat absorbed on NPs was eluted using NaOH and ascorbic acid. Upon optimization, paraquat could be...

  3. Electrospray ionization-ion mobility spectrometry as a detection system for three-phase hollow fiber microextraction technique and simultaneous determination of trimipramine and desipramine in urine and plasma samples.

    Science.gov (United States)

    Jafari, M T; Saraji, M; Sherafatmand, H

    2011-04-01

    A novel method based on three-phase hollow fiber microextraction technique (HF-LPME) coupled with electrospray ionization-ion mobility spectrometry (ESI-IMS) was developed for the simultaneous determination of two antidepressant drugs (trimipramine and desipramine) in urine and plasma samples. The effects of various parameters such as type of organic solvent, composition of donor and acceptor phase, stirring rate, salt addition, extraction time, and temperature were investigated. Under the optimized conditions, the relative standard deviation was in the range of 5-6%, and the method quantitation limit (MQL) of utilizing HF-LPME/ESI-IMS was 5 μg/L for both drugs. The relative recoveries obtained by the proposed method from urine and plasma samples were in the range 94% to 97% for trimipramine and 92% to 96% for desipramine. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of trace amounts of trimipramine and desipramine in biological samples without any significant matrix effect.

  4. Development and validation of a sensitive liquid chromatographic-tandem mass spectrometric method for the simultaneous analysis of granisetron and 7-hydroxy granisetron in human plasma and urine samples: application in a clinical pharmacokinetic study in pregnant subject.

    Science.gov (United States)

    Zhao, Yang; Chen, Hui-Jun; Caritis, Steve; Venkataramanan, Raman

    2016-02-01

    A liquid chromatography-tandem mass spectrometric method for the quantification of granisetron and its major metabolite, 7-hydroxy granisetron in human plasma and urine samples was developed and validated. Respective stable isotopically labeled granisetron and 7-hydroxy granisetron were used as internal standards (IS). Chromatography was performed using an Xselect HSS T3 analytical column with a mobile phase of 20% acetonitrile in water (containing 0.2 mM ammonium formate and 0.14% formic acid, pH 4) delivered in an isocratic mode. Tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring was used for quantification. The standard curves were linear in the concentration ranges of 0.5-100 ng/mL for granisetron and 0.1-100 ng/mL for 7-hydroxy granisetron in human plasma samples, and 2-2000 ng/mL for granisetron and 2-1000 ng/mL for 7-hydroxy granisetron in human urine samples, respectively. The accuracies were >85% and the precision as determined by the coefficient of variations was validated method was successfully applied to a pharmacokinetic study after intravenous administration of 1 mg granisetron to a pregnant subject.

  5. Application of molecular imprinted polymer nanoparticles as a selective solid phase extraction for preconcentration and trace determination of 2,4-dichlorophenoxyacetic acid in the human urine and different water samples.

    Science.gov (United States)

    Omidi, Fariborz; Behbahani, Mohammad; Sadeghi Abandansari, Hamid; Sedighi, Alireza; Shahtaheri, Seyed Jamaleddin

    2014-01-01

    A molecular-imprinted polymer nanoparticles (MIP-NP) for the selective preconcentration of 2,4-dichlorophenoxyacetic acid (2,4-D) is described. It was obtained by precipitation polymerization from methacrylic acid (the functional monomer), ethylene glycol dimethacrylate (the cross-linker), 2,2'-azobisisobutyronitrile (the initiator) and 2,4-D (the template molecule) in acetonitrile solution. The MIP-NPs were characterized by thermogravimetric analysis, and by scanning electron microscopy. Imprinted 2,4-D molecules were removed from the polymeric structure using acetic acid in methanol (15:85 v/v %) as the eluting solvent. The sorption and desorption process occur within 10 min and 15 min, respectively. The maximum sorbent capacity of the molecular imprinted polymer is 89.2 mg g(-1). The relative standard deviation and limit of detection for water samples by introduced selective solid phase extraction were 4.2% and 1.25 μg L(-1), and these data for urine samples were 4.7% and 1.80 μg L(-1), respectively. The method was applied to the determination of 2,4-D in the urine and different water samples.

  6. Metabonomics and population studies: age-related amino acids excretion and inferring networks through the study of urine samples in two Italian isolated populations.

    Science.gov (United States)

    D'Adamo, Pio; Ulivi, Sheila; Beneduci, Amerigo; Pontoni, Gabriele; Capasso, Giovambattista; Lanzara, Carmela; Andrighetto, Gilberto; Hladnik, Uros; Nunes, Virginia; Palacin, Manuel; Gasparini, Paolo

    2010-01-01

    The study of two different Italian isolated populations was combined with a metabonomic approach to better understand tubular handling of amino acids. Levels of amino acids and metabolites have been analyzed by Nucleic Magnetic Resonance and expressed as ratio vs urinary creatinine concentration (mmol/mol). For most of the amino acids there is an age-related U shape pattern of excretion, with the peaks during childhood and old age, and a significant reduction in the adult age. Hierarchical cluster analysis has clearly identified three groups clustering the same amino acids: His, Thr and Ala (group one); Gly and Phe (group two) and a third larger one. Results have been further confirmed by factor and regression analysis, and used to confirm and, in some cases, infer new amino acids networks. As a matter of facts, the identification of strong evidences for clustering of urine excretion of several neutral amino acids suggests the predominant impact of relevant and common transporters.

  7. Simultaneous determination of 11 antibiotics and their main metabolites from four different groups by reversed-phase high-performance liquid chromatography-diode array-fluorescence (HPLC-DAD-FLD) in human urine samples.

    Science.gov (United States)

    Fernandez-Torres, R; Consentino, M Olías; Lopez, M A Bello; Mochon, M Callejon

    2010-05-15

    A new, accurate and sensitive reversed-phase high-performance liquid chromatography (RP-HPLC) as analytical method for the quantitative determination of 11 antibiotics (drugs) and the main metabolites of five of them present in human urine has been worked out, optimized and validated. The analytes belong to four different groups of antibiotics (sulfonamides, tetracyclines, penicillins and anphenicols). The analyzed compounds were sulfadiazine (SDI) and its N(4)-acetylsulfadiazine (NDI) metabolite, sulfamethazine (SMZ) and its N(4)-acetylsulfamethazine (NMZ), sulfamerazine (SMR) and its N(4)-acetylsulfamerazine (NMR), sulfamethoxazole (SMX), trimetroprim (TMP), amoxicillin (AMX) and its main metabolite amoxicilloic acid (AMA), ampicillin (AMP) and its main metabolite ampicilloic acid (APA), chloramphenicol (CLF), thiamphenicol (TIF), oxytetracycline (OXT) and chlortetracycline (CLT). For HPLC analysis, diode array (DAD) and fluorescence (FLD) detectors were used. The separation of the analyzed compounds was conducted by means of a Phenomenex Gemini C(18) (150mm x 4.6mm I.D., particle size 5microm) analytical column with LiChroCART LiChrospher C(18) (4mm x 4mm, particle size 5microm) guard column. Analyzed drugs were determined within 34min using formic acid 0.1% in water and acetonitrile in gradient elution mode as mobile phase. A linear response was observed for all compounds in the range of concentration studied. Two procedures were optimized for sample preparation: a direct treatment with methanol and acetonitrile and a solid phase extraction procedure using Bond Elut Plexa columns. The method was applied to the determination of the analytes in human urine from volunteers under treatment with different pharmaceutical formulations. This method can be successfully applied to routine determination of all these drugs in human urine samples.

  8. Dispersive liquid-liquid microextraction based on solidification of floating organic drop combined with field-amplified sample injection in capillary electrophoresis for the determination of beta(2)-agonists in bovine urine.

    Science.gov (United States)

    Us, Murat Faruk; Alshana, Usama; Lubbad, Ibrahim; Göğer, Nilgün G; Ertaş, Nusret

    2013-03-01

    Dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) was for the first time combined with field-amplified sample injection (FASI) in CE to determine four β(2)-agonists (cimbuterol, clenbuterol, mabuterol, and mapenterol) in bovine urine. Optimum BGE consisted of 20 mM borate buffer and 0.1 mM SDS. Using salting-out extraction, β(2)-agonists were extracted into ACN that was then used as the disperser solvent in DLLME-SFO. Optimum DLLME-SFO conditions were: 1.0 mL ACN, 50 μL 1-undecanol (extraction solvent), total extraction time 1.5 min, no salt addition. Back extraction into an aqueous solution (pH 2.0) facilitated direct injection of β(2)-agonists into CE. Compared to conventional CZE, DLLME-SFO-FASI-CE achieved sensitivity enhancement factors of 41-1046 resulting in LODs in the range of 1.80-37.0 μg L(-1). Linear dynamic ranges of 0.15-10.0 mg L(-1) for cimbuterol and 15-1000 μg L(-1) for the other analytes were obtained with coefficients of determination (R(2)) ≥ 0.9901 and RSD% ≤5.5 (n = 5). Finally, the applicability of the proposed method was successfully confirmed by determination of the four β(2)-agonists in spiked bovine urine samples and accuracy higher than 96.0% was obtained.

  9. Comparison of dispersive liquid-liquid microextraction based on organic solvent and ionic liquid combined with high-performance liquid chromatography for the analysis of emodin and its metabolites in urine samples.

    Science.gov (United States)

    Tian, Jie; Chen, Xuan; Bai, Xiaohong

    2012-01-01

    In this paper, two methods based on organic solvent dispersive liquid-liquid microextraction (OS-DLLME) and ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) coupled with high-performance liquid chromatography have been critically compared for analyzing emodin and its metabolites (aloe-emodin, anthraquinone-2-carboxylic acid, rhein, danthron, chrysophanol and physcion) in urine samples. Several important parameters influencing the extraction recoveries of DLLME were carefully optimized. Under optimal conditions, the enrichment factors (EFs) for emodin and its metabolites by OS-DLLME and IL-DLLME were within the range of 90-295 and 63-192 respectively; the relative standard deviations (RSDs, n=3) for intra-day and inter-day precision were lower than 7.2 and 8.7% by OS-DLLME, and lower than 5.7 and 6.4% by IL-DLLME; the recoveries of emodin and its metabolites were from 87.1 to 105% for OS-DLLME and from 94.8 to 103% for IL-DLLME, respectively. There were no significant deviations between the two methods for the determination of emodin and its metabolites. From the results of HPLC/UV of urine sample after DLLME, the metabolites aloe-emodin, rhein, chrysophanol and physcion were identified by comparing the retention times with the standards. From the results of HPLC/MS, anthraquinone-2-carboxylic acid and danthron as unreported metabolites of emodin were found.

  10. Magnetic Solid-Phase Extraction Using Fe3O4@SiO2 Magnetic Nanoparticles Followed by UV-Vis Spectrometry for Determination of Paraquat in Plasma and Urine Samples.

    Science.gov (United States)

    Sha, Ou; Wang, Yu; Yin, Xin; Chen, Xiaobing; Chen, Li; Wang, Shujun

    2017-01-01

    A rapid and simple method was optimized and validated for the separation and quantification of paraquat, a frequently used herbicide and a leading cause of fatal poisoning worldwide, at trace levels with UV-Vis spectrophotometry in plasma and urine samples by direct magnetic solid-phase extraction. Fe3O4@SiO2 nanoparticles (NPs) were used as the magnetic solid-phase extraction agents and the paraquat absorbed on NPs was eluted using NaOH and ascorbic acid. Upon optimization, paraquat could be extracted and concentrated from various samples by 35-fold. The linear range, limit of detection (LOD), correlation coefficient (R), and relative standard deviation (RSD) could reach 15.0-400.0 μg/L, 12.2 μg/L, 0.9987, and 0.65% (n = 5, c = 40.0 μg/L), respectively. The Fe3O4@SiO2 NPs could be reused up to five times. The method was successfully applied to the determination of paraquat in urine and plasma at different hemoperfusion numbers in a local hospital for the patient of paraquat poisoning. The experiment result could not only enable immediate medical intervention but also benefit patients' survival.

  11. Magnetic Solid-Phase Extraction Using Fe3O4@SiO2 Magnetic Nanoparticles Followed by UV-Vis Spectrometry for Determination of Paraquat in Plasma and Urine Samples

    Directory of Open Access Journals (Sweden)

    Ou Sha

    2017-01-01

    Full Text Available A rapid and simple method was optimized and validated for the separation and quantification of paraquat, a frequently used herbicide and a leading cause of fatal poisoning worldwide, at trace levels with UV-Vis spectrophotometry in plasma and urine samples by direct magnetic solid-phase extraction. Fe3O4@SiO2 nanoparticles (NPs were used as the magnetic solid-phase extraction agents and the paraquat absorbed on NPs was eluted using NaOH and ascorbic acid. Upon optimization, paraquat could be extracted and concentrated from various samples by 35-fold. The linear range, limit of detection (LOD, correlation coefficient (R, and relative standard deviation (RSD could reach 15.0–400.0 μg/L, 12.2 μg/L, 0.9987, and 0.65% (n=5, c = 40.0 μg/L, respectively. The Fe3O4@SiO2 NPs could be reused up to five times. The method was successfully applied to the determination of paraquat in urine and plasma at different hemoperfusion numbers in a local hospital for the patient of paraquat poisoning. The experiment result could not only enable immediate medical intervention but also benefit patients’ survival.

  12. MALDI-TOF MS 在中段尿样本细菌直接检测中的应用%Application of MALDI-TOF MS for identifying bacteria directly in midstream urine samples

    Institute of Scientific and Technical Information of China (English)

    王琳; 李佳萍; 陈功祥; 张嵘

    2015-01-01

    目的:运用基质辅助激光解析电离飞行时间质谱(MALDI-TOF MS )鉴定系统对中段尿样本中的细菌进行直接快速检测,以建立快速的细菌检测方法便于临床应用。方法692例中段尿样本接种于固体培养基上,利用 MALDI-TOF MS 和 Vitek 2 Compact 全自动微生物分析系统(简称 Vitek 2 Compact)对单个菌落进行鉴定;同时对尿液样本进行前处理后直接进行质谱分析。结果692例中段尿样本中,98例单一菌感染且细菌数>104 CFU /mL 的样本应用 MALDI-TOF MS 直接检测出74株菌,检出率达75.5%,其中大肠埃希菌39株,检出率达79.6%;粪肠球菌23株,检出率为100.0%;摩根摩根菌5株,检出率为100.0%。64例样本为2种菌混合感染,采用 MALDI-TOF MS 直接检测出44例样本中的1种优势细菌。质谱直接检测尿液的鉴定结果与单菌落质谱鉴定结果及 Vitek 2 Compact 鉴定结果完全一致,符合率为100.0%。结论MALDI-TOF MS 可用于直接检测尿液样本中的细菌,检出率高,结果可靠;MALDI-TOF MS 对混合菌感染的样本有一定鉴定能力;该方法可比常规尿培养鉴定方法提早42 h 报告鉴定结果,是对临床尿液样本细菌鉴定的一大革命性进步。%Objective To construct rapid identification method for clinical laboratory with the use of matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF MS)for the direct identification of bacteria in midstream urine samples.Methods A total of 692 midstream urine samples were cultivated on agar,and were identified by MALDI-TOF MS and Vitek 2 Compact automated microbial amalyslis system (Vitek 2 Compact ). Direct identification of midstream urine samples were also conducted by MALDI-TOF MS after preparation.Results Of the 692 midstream urine samples,98 samples were positive for one kind of bacteria (>1 04 CFU /mL).The overall detection rate of direct

  13. Murine Automated Urine Sampler (MAUS) Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This proposal outlines planned development for a low-power, low-mass automated urine sample collection and preservation system for small mammals, capable of...

  14. Highly sensitive trivalent copper chelate–luminol chemiluminescence system for capillary electrophoresis chiral separation and determination of ofloxacin enantiomers in urine samples

    Directory of Open Access Journals (Sweden)

    Hao-Yue Xie

    2014-12-01

    Full Text Available A simple, fast and sensitive capillary electrophoresis (CE strategy combined with chemiluminescence (CL detection for analysis of ofloxacin (OF enantiomers was established in the present work. Sulfonated β-cyclodextrin (β-CD was used as the chiral additive being added into the running buffer of luminol–diperiodatocuprate (III (K5[Cu(HIO62], DPC chemiluminescence system. Under the optimum conditions, the proposed method was successfully applied to separation and analysis of OF enantiomers with the detection limits (S/N=3 of 8.0 nM and 7.0 nM for levofloxacin and dextrofloxacin, respectively. The linear ranges were both 0.010–100 μM. The method was utilized for analyzing OF in urine; the results obtained were satisfactory and recoveries were 89.5–110.8%, which demonstrated the reliability of this method. This approach can also be further extended to analyze different commercial OF medicines.

  15. pH-resistant titania hybrid organic-inorganic coating for stir bar sorptive extraction of drugs of abuse in urine samples followed by high performance liquid chromatography-ultraviolet visible detection.

    Science.gov (United States)

    Lan, Lidan; Hu, Bin; Yu, Chunhe

    2010-11-05

    An organic-inorganic hybrid titania-hydroxy-terminated silicone oil (titania-OH-TSO) stir bar coating was prepared by sol-gel method. The extraction performance of titania-OH-TSO coated stir bar was evaluated and compared with poly(dimethysiloxane) (PDMS), poly(dimethysiloxane)-divinylbenzene (PDMS-DVB), poly(dimethysiloxane)-β-cyclodextrin (PDMS-β-CD) and C(18) coated stir bar with five polar drugs of abuse including amphetamine (PA), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and ketamine (Ke) as the model analytes. The experimental results revealed that the titania-OH-TSO coated stir bar exhibited highly pH-resistant ability, good preparation reproducibility, superior selectivity and high extraction efficiency for the target compounds. Based on this fact, a new method of titania-OH-TSO coated stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet visible (UV) detection was developed for the analysis of five drugs of abuse in urine samples. The factors affecting the extraction efficiency of SBSE such as sample pH, desorption solvent, sample volume, extraction time, desorption time, stirring rate and ionic strength were investigated and the optimal extraction conditions were established. Under the optimized conditions, the limits of detection (LODs) for titania-OH-TSO coated SBSE-HPLC-UV determination of five polar drugs of abuse were in the range of 2.3-9.1 μg/L with relative standard deviations (RSDs) ranging from 7.3 to 8.9% (c=300 μg/L, n=6), and all of the target compounds exhibited good linearity over a concentration range of 30-3000 μg/L. The developed method was applied to the determination of amphetamines and Ke in urine samples of drug abusers with satisfactory results.

  16. HPV testing in first-void urine provides sensitivity for CIN2+ detection comparable with a smear taken by a clinician or a brush-based self-sample: cross-sectional data from a triage population.

    Science.gov (United States)

    Leeman, A; Del Pino, M; Molijn, A; Rodriguez, A; Torné, A; de Koning, M; Ordi, J; van Kemenade, F; Jenkins, D; Quint, W

    2017-08-01

    To compare the sensitivity of high-risk human papillomavirus (hrHPV) and genotype detection in self-collected urine samples in the morning (U1), and later on (U2), brush-based self-samples (SS), and clinician-taken smears (CTS) for detecting cervical intraepithelial neoplasia grade 2+ (CIN2+) in a colposcopic referral population. Cross-sectional single-centre study. A colposcopy clinic in Spain. A cohort of 113 women referred for colposcopy after an abnormal Pap smear. Women undergoing colposcopy with biopsy for abnormal Pap smears were sent a device (Colli-Pee™, Novosanis, Wijnegem, Belgium) to collect U1 on the morning of colposcopy. U2, CTS, and SS (Evalyn brush™, Rovers Medical Devices B.V., Oss, the Netherlands) were also analysed. All samples were tested for HPV DNA using the analytically sensitive SPF10-DEIA-LiPA25 assay and the clinically validated GP5+/6+-EIA-LMNX. Histologically confirmed CIN2+ and hrHPV positivity for 14 high-risk HPV types. Samples from 91 patients were analysed. All CIN3 cases (n = 6) tested positive for hrHPV in CTS, SS, U1, and U2 with both HPV assays. Sensitivity for CIN2+ with the SPF10 system was 100, 100, 95, and 100%, respectively. With the GP5+/6+ assay, sensitivity was 95% in all sample types. The sensitivities and specificities for both tests on each of the sample types did not significantly differ. There was 10-14% discordance on hrHPV genotype. CIN2+ detection using HPV testing of U1 shows a sensitivity similar to that of CTS or brush-based SS, and is convenient. There was substantial to almost excellent agreement between all samples on genotype with both hrHPV assays. There was no advantage in testing U1 compared with U2 samples. Similar CIN2+ sensitivity for HPV testing in first-void urine, physician-taken smear and brush-based self-sample. © 2017 Royal College of Obstetricians and Gynaecologists.

  17. 肠球菌感染分布及其耐药性分析%Analysis of enterococcus infection distribution and drug resistance in urine sample

    Institute of Scientific and Technical Information of China (English)

    任玲龙; 宣迎梅

    2014-01-01

    Objective To understand enterococcus distribution in hospitalized patients with urinary tract infec‐tion and drug resistance characteristic ,provide the basis for clinical diagnosis and treatment .Methods In our hospital from January 2011 to December 2011 ,enterococcus strains from clinical urine culture were identified ,drug sensitive experiment were operated by the method of K‐B .The results were judged according to the standard of CLSI2010 . The data were analyzed by WHONET5 .5 softwareResults Enterococcus Faecium and Enterococcus faecalis was more seen in 253 cases of enterococcus in patients with urinary tract infection ,59 .7% and 38 .7% ,respectively .The drug resistance of Enterococcus Faecium in high concentration of gentamicin ,penicillin kind ,nitrofurantoin ,quinolone were significantly higher than that of dung enterococcus ,the resistant strains to vancomycin were urine enterococcus ,the resistant rate was 2 .04% .All of enterococcus were sensitive to rina thiazole amine ,the rate was 100% ,the sen‐sitive rate of enterococcus to theTeicoplanin was 98 .8% ,but ,the sensitive rate of its to levofloxacin was only 32 .1%.Conclusion The whole of enterococcus resistance has become increasingly serious .The found of vancomycin resist‐ant of enterococcus could be used as the guidance for clinical medication .%目的:为了解该院住院患者泌尿系感染中的肠球菌分布特点及耐药特征,为临床诊断和治疗提供依据。方法对该院2011年1月至2012年12月临床尿液标本培养分离鉴定,采用K‐B法对分离到的肠球菌进行药敏实验,结果判读依据CLSI2010标准,用WHONET5.5软件进行数据分析。结果253例肠球菌泌尿系感染患者中以粪肠球菌和屎肠球菌为多见,分别为59.7%和38.7%。屎肠球菌对高浓度庆大霉素、青霉素类、呋喃妥因、喹诺酮类耐药性明显高于粪肠球菌,耐万古霉素的全为屎肠球菌,耐药率为2.04%。但

  18. The influence Bladder Training Initiation to the Urine Residual of Stroke Patients with Urine Catheter

    Directory of Open Access Journals (Sweden)

    Wahyu Hidayati

    2011-07-01

    Full Text Available ABSTRACT The stroke patients usually experience with various dysfunction, including disturbance in elimination because of neurogenic bladder. Urine residue can be used to detect the bladder function in contracting and voiding urine. This research was aimed to compare bladder training initiation after stroke patients have passed the acute phase and one day before the urine catheter was removal. This research was used Quasy experiment posttest-only design with a comparison group design. The sample in this research taking by purposive random sampling method. Urine residue measuring with bladder scan and recorded in the observation sheet. The mean of urine residue in the treatment group was smaller (54,00 ml with SD=144,22 ml if compared with the urine residue volume in control group (101,71 ml with SD=42,55 ml. The influence bladder training in both of treatment and control groups and the differences of the urine residue volume was analyzed with t test independent, there wes no differences between urine residue volume in the groups (p=0,84. Therefore the health institution must consider to develop the system and made a procedure in bladder training program’s and the nurse must do bladder training before the urine catheter was removal. Keywords: bladder training, stroke patient, neurogenic bladder, nurse

  19. On-Demand Urine Analyzer

    Science.gov (United States)

    Farquharson, Stuart; Inscore, Frank; Shende, Chetan

    2010-01-01

    A lab-on-a-chip was developed that is capable of extracting biochemical indicators from urine samples and generating their surface-enhanced Raman spectra (SERS) so that the indicators can be quantified and identified. The development was motivated by the need to monitor and assess the effects of extended weightlessness, which include space motion sickness and loss of bone and muscle mass. The results may lead to developments of effective exercise programs and drug regimes that would maintain astronaut health. The analyzer containing the lab-on-a- chip includes materials to extract 3- methylhistidine (a muscle-loss indicator) and Risedronate (a bone-loss indicator) from the urine sample and detect them at the required concentrations using a Raman analyzer. The lab-on- a-chip has both an extractive material and a SERS-active material. The analyzer could be used to monitor the onset of diseases, such as osteoporosis.

  20. Comparison of routine urinalysis and urine Gram stain for detection of bacteriuria in dogs.

    Science.gov (United States)

    Way, Leilani Ireland; Sullivan, Lauren A; Johnson, Valerie; Morley, Paul S

    2013-01-01

    To determine the utility of performing urine Gram stain for detection of bacteriuria compared to routine urine sediment examination and bacterial aerobic urine culture. Prospective, observational study. University teaching hospital. Urine samples acquired via cystocentesis through convenience sampling from 103 dogs presenting to a tertiary referral institution. All samples underwent routine urinalysis, including sediment examination, as well as urine Gram stain and quantitative bacterial aerobic urine culture. The urine Gram stain demonstrated improved sensitivity (96% versus 76%), specificity (100% versus 77%), positive predictive value (100% versus 83%), and negative predictive value (93% versus 69%) when identifying bacteriuria, compared to routine urine sediment examination. The urine Gram stain is highly sensitive and specific when detecting the presence of bacteria in canine urine samples. Gram staining should be considered when bacteriuria is highly suspected and requires rapid identification while bacterial culture is pending. © Veterinary Emergency and Critical Care Society 2013.

  1. Evaluation of the results of Mycobacterium tuberculosis direct test (MTD and Mycobacterial culture in urine samples Avaliação de resultados do Teste Direto para Mycobacterium tuberculosis (MTD e da cultura para micobacterias em amostras de urina

    Directory of Open Access Journals (Sweden)

    Asli Gamze Sener

    2008-12-01

    Full Text Available Tuberculosis remains a public health problem in Turkey. Rapid detection of Mycobacterium tuberculosis plays a key role in control of infection. In this article, the Gen-Probe Amplified Mycobacterium Tuberculosis Direct Test (MTD was evaluated for detection of M. tuberculosis in urine samples. The performance of the MTD was very good and appropriate for routine laboratory diagnosis.A tuberculose continua sendo um problema de saúde pública na Turquia. A detecção rápida de Mycobacterium tuberculosis tem um papel importante no controle da infecção. Nesse artigo, avaliou-se o Gen-Probe Amplified Mycobacterium Tuberculosis Test (MTD para detecção de M. tuberculosis em amostras de urina. O desempenho do MTD foi muito bom e adequado para diagnóstico laboratorial de rotina.

  2. Distribution and resistance analysis of pathogens from in-patients urine samples%住院患者尿标本病原菌的分布特点及耐药性分析

    Institute of Scientific and Technical Information of China (English)

    虞丹丹; 周翠; 刘媚娜; 李少禧; 周铁丽

    2011-01-01

    目的:了解住院患者尿液标本病原菌的分布特点及耐药性分析,指导临床合理使用抗菌药物.方法:对2010年1月-2010年11月,我院住院患者尿液标本病原菌的分布特点及抗菌药物敏感性进行回顾性分析.结果:2346份中段尿标本中,阳性率较高的科室是神经内科、脑血管科及ICU.748株非重复菌株以大肠埃希菌最为多见,占30.9%,产ES-BLs的大肠埃希菌及肺炎克雷伯菌的检出率为52.4%;多种革兰阴性杆菌呈现出多重耐药现象.耐甲氧西林表皮葡萄球菌的检出率(85.7%)高于耐甲氧西林金黄色葡萄球菌的检出率(35.3%);屎肠球菌耐药现象较粪肠球菌严重,并发现2株耐万古霉素的屎肠球菌.真菌感染以白色念珠菌多见,占39.5%,尚未发现对两性霉素B及5-氟胞嘧啶的耐药菌株.结论:尿路感染病原菌分布广泛,大肠埃希菌是尿路感染的优势菌种,多种菌株已呈现出多重耐药现象,临床医生需根据具体药敏结果,合理选择抗菌药物,尽量减少耐药菌株的出现.%Objective:To investigate the distribution and drug resistance analysis of pathogens isolated from in -patients urine samples for the guidance of rational using antibiotics. Methods: A retrospective analysis was made about distribution and drug sensitivity of pathogens from in - patients urine samples from Jan 2010 to Nov 2010. Results: Neurology, brain vessel division and ICU were composed higher positive rate from 2346 samples. The most common pathogen was Escherichia coli( 30.9% ) in 748 unrepeated pathogens. The positive rate of ESBLs in Escherichia coli and Klebsiella pneumoniae was 52.4%. The phenomena of multi - drug - resistance was founded in various gram negative bacillus. The detection rate of meticillin - resistance Staphylococcus epidermis ( 85.7% ) was higher than the S. aureus ( 35.3% ). The drug - resistance of Enterococcus faecium was more serious than Enterococcusfaecalis, and vancomycin

  3. Urine testing for diabetic analysis

    Directory of Open Access Journals (Sweden)

    Janet Marsden

    2016-04-01

    Full Text Available Urine testing is relatively cheap and easy to do. Urine testing can be used to check for blood in the urine, to check for infection (by detecting the presence of white blood cells or protein and can show up other systemic problems such as liver problems (by showing abnormal bilirubin levels. Urine testing can also detect ketones in the urine.

  4. Molecularly imprinted-solid phase extraction combined with simultaneous derivatization and dispersive liquid-liquid microextraction for selective extraction and preconcentration of methamphetamine and ecstasy from urine samples followed by gas chromatography.

    Science.gov (United States)

    Djozan, Djavanshir; Farajzadeh, Mir Ali; Sorouraddin, Saeed Mohammad; Baheri, Tahmineh

    2012-07-27

    In this study, a developed technique was reported for extraction and pre-concentration of methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA, ecstasy) from urine samples using molecularly imprinted-solid phase extraction (MISPE) along with simultaneous derivatization and dispersive liquid-liquid microextraction (DLLME). Molecularly imprinted microspheres as sorbent in solid phase extraction (SPE) procedure were synthesized using precipitation polymerization with MAMP as the template. Aqueous solution of the target analytes was passed through MAMP-MIP cartridge and the adsorbed analytes were then eluted with methanol. The collected eluate was mixed with butylchloroformate which served as the derivatization reagent as well as the extraction solvent. The mixture was immediately injected into deionized water. After centrifugation, 1 μL of the settled organic phase was injected into gas chromatography-flame ionization detection (GC-FID) or gas chromatography-mass spectrometry (GC-MS). Various experimental parameters affecting the performance of both of the steps (MISPE and DLLME) were thoroughly investigated. The calibration graphs were linear in the ranges of 10-1500 ng mL(-1) (MAMP) and 50-1500 ng mL(-1) (MDMA), and the detection limits (LODs) were 2 and 18 ng mL(-1), respectively. The relative standard deviations (%RSDs) obtained for six repeated experiments (100 ng mL(-1) of each drug) were 5.1% and 6.8% for MAMP and MDMA, respectively. The relative recoveries obtained for the analytes in human urine samples, spiked with different levels of each drug, were within the range of 80-88%.

  5. Efficiency of a miniaturized silica monolithic cartridge in reducing matrix ions as demonstrated in the simultaneous extraction of morphine and codeine from urine samples for quantification with liquid chromatography-tandem mass spectrometry (LC-MS/MS).

    Science.gov (United States)

    Nema, T; Chan, E C Y; Ho, P C

    2011-09-01

    Presence of matrix ions could negatively affect the sensitivity and selectivity of liquid chromatography-tandem mass spectrometer (LC-MS/MS). In this study, the efficiency of a miniaturized silica monolithic cartridge in reducing matrix ions was demonstrated in the simultaneous extraction of morphine and codeine from urine samples for quantification with LC-MS. The miniaturized silica monolith with hydroxyl groups present on the largely exposed surface area function as a weak cation exchanger for solid phase extraction (SPE). The miniaturized silica cartridge in 1 cm diameter and 0.5 cm length was housed in a 2-ml syringe fixed over a SPE vacuum manifold for extraction. The cleaning effectiveness of the cartridge was confirmed by osmometer, atomic absorption spectrometer, LC-MS and GC-TOFMS. The drugs were efficiently extracted from urine samples with recoveries ranging from 86% to 114%. The extracted analytes, after concentration and reconstitution, were quantified using LC-MS/MS. The limits of detection for morphine and codeine were 2 ng/ml and 1 ng/mL, respectively. The relative standard deviations of measurements ranged from 3% to 12%. The monolithic sorbent offered good linearity with correlation coefficients > 0.99, over a concentration range of 50-500 ng/ml. The silica monolithic cartridge was found to be more robust than the particle-based packed sorbent and also the commercial cartridge with regards to its recyclability and repeated usage with minimal loss in efficiency. Our study demonstrated the efficiency of the miniaturized silica monolith for removal of matrix ions and extraction of drugs of abuse in urinary screening.

  6. Pink urine syndrome

    Directory of Open Access Journals (Sweden)

    Luis del Carpio-Orantes

    2017-03-01

    Full Text Available In the present images we allude to a syndrome of low incidence, characterized by pink urine, being related to factors such as obesity, and being triggered by abdominal surgeries, use of propofol, among others. Being favoured by the presence of abundant crystals of uric acid in the urine confers the typical pink coloration.

  7. Mutagens in urine of carbon electrode workers

    Energy Technology Data Exchange (ETDEWEB)

    Pasquini, R.; Monarca, S.; Sforzolini, G.S.; Conti, R.; Fagioli, F.

    1982-01-01

    Following previous work carried out in an Italian factory producing carbon electrodes and evaluating the occupational mutagenic-carcinogenic hazards, the authors studied the presence of mutagen metabolites in the urine of workers in the same factory who were exposed to petroleum coke and pitch and in the urine of a control group of unexposed workers. The urine samples were concentrated by absorption on XAD-2 columns and were tested using the Salmonella/microsome assay (strain TA98, TA100, TA1535, TA1538) with and without the addition of beta-glucuronidase and metabolizing system. The collection of urine samples was carried out twice, with an interval of 2 months; 'before working time', 'after working time', and also during Sunday. The results showed that urine samples collected 'before' occupational exposure (upon waking) or on Sunday revealed no mutagenic activity in either worker groups and that the urine samples collected after or during occupational exposure revealed high mutagenic activity in the exposed workers, with a statistically significant difference between the mean of the revertants/plate values for exposed and unexposed workers. On the basis of the previous and the present research, the authors suggest that application of the Salmonella/microsome test to work environments could offer useful and suitable tool for evaluating the health hazards due to mutagenic/carcinogenic substances from occupational exposure.

  8. Perbandingan kandungan iodium dalam urin antara sampel urin 24 jam dan on spot pada anak usia sekolah

    Directory of Open Access Journals (Sweden)

    Widya Ayu Kurnia Putri

    2017-01-01

    Full Text Available Background: Urine Iodine Concentration (UIC is the indicator to assess iodine status. UIC from 24-hour urine collection appropriate to used as a direct measure of the iodine status and helps to validate the estimates intake of iodine. 24-hours urine collection is not practical in large studies and epidemiological surveys because it is quite difficult to complete and accurate collection. WHO/UNICEF/ICCIDD recommend the use of on spot urine collection. Objective: The aim of this study was to compare of 24-hour urine collection and spot urine collection for the assessment UIC in children. Method: The cross-sectional study was applied in Bogor. UIC was measured in 24-hour urine and parallel collected three spot urine namely on spot 1 collected morning, on spot 2 collected afternoon, and on spot 3 collected evening, sample urine collected from 44 healthy children age 10-13 years. UIC of 24-hour urine and one spot urine analyzed in the laboratory GAKY FK UNDIP using acid digestion method. Results: The average UIC from 24-hour urine collection was 179.77 ± 56.4 µg/l and UIC from on spot urine collection were on spot morning 145.30 ± 63.6 µg/l, on spot afternoon 159.95 ± 64.5 µg/l, and on spot evening 167.50 ± 66.1 µg/l. However, UIC correlation between UIC from on spot afternoon and UIC 24-hour (r = 0.456 with 66.67 % sensitivity and 75.61 % specificity. Conclusion: UIC urine samples from lunch to dinner more accurately reflects the UIC 24 hours to categorize the iodine status of the population. UIC from spot urine samples collected on the afternoon can be used as an alternative to evaluate the iodine status of school-age children.

  9. Primary culture media for routine urine processing.

    OpenAIRE

    Fung, J C; Lucia, B; Clark, E.; Berman, M.; Goldstein, J.; D'Amato, R F

    1982-01-01

    It has been recommended that routine microbiological processing of urine specimens include quantitative plating onto blood agar medium along with a selective and differential agar such as MacConkey agar for gram-negative organisms. Few data have been published to justify this combination. To evaluate the validity of this recommendation 2,553 midstream, clean-voided urine samples were quantitatively plated onto blood agar, MacConkey agar, and colistin-nalidixic acid agar, which is a selective ...

  10. Blood in the Urine (Hematuria)

    Science.gov (United States)

    ... of Healthy Breakfasts Shyness Blood in the Urine (Hematuria) KidsHealth > For Teens > Blood in the Urine (Hematuria) ... español Sangre en la orina (hematuria) What Is Hematuria? When blood gets into a person's urine (pee), ...

  11. Achieving second order advantage with multi-way partial least squares and residual bi-linearization with total synchronous fluorescence data of monohydroxy-polycyclic aromatic hydrocarbons in urine samples.

    Science.gov (United States)

    Calimag-Williams, Korina; Knobel, Gaston; Goicoechea, H C; Campiglia, A D

    2014-02-06

    An attractive approach to handle matrix interference in samples of unknown composition is to generate second- or higher-order data formats and process them with appropriate chemometric algorithms. Several strategies exist to generate high-order data in fluorescence spectroscopy, including wavelength time matrices, excitation-emission matrices and time-resolved excitation-emission matrices. This article tackles a different aspect of generating high-order fluorescence data as it focuses on total synchronous fluorescence spectroscopy. This approach refers to recording synchronous fluorescence spectra at various wavelength offsets. Analogous to the concept of an excitation-emission data format, total synchronous data arrays fit into the category of second-order data. The main difference between them is the non-bilinear behavior of synchronous fluorescence data. Synchronous spectral profiles change with the wavelength offset used for sample excitation. The work presented here reports the first application of total synchronous fluorescence spectroscopy to the analysis of monohydroxy-polycyclic aromatic hydrocarbons in urine samples of unknown composition. Matrix interference is appropriately handled by processing the data either with unfolded-partial least squares and multi-way partial least squares, both followed by residual bi-linearization.

  12. Restricted accessed material-copper(II) ion imprinted polymer solid phase extraction combined with inductively coupled plasma-optical emission spectrometry for the determination of free Cu(II) in urine and serum samples.

    Science.gov (United States)

    Cui, Chao; He, Man; Chen, Beibei; Hu, Bin

    2013-11-15

    A novel restricted accessed material (RAM)-Cu(II) ion imprinted polymer (IIP) was synthesized by the surface imprinted-emulsion method, and possessed a high selectivity to Cu(II) and good macromolecules exclusion property. And a novel method of RAM-IIP packed microcolumn solid phase extraction (SPE) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the determination of trace free Cu(II) in human body fluids. Under the optimized conditions, the adsorption capacity of RAM-IIP for Cu(II) was 15.9 mg g(-1). With a preconcentration factor of 30, the limit of detection was 0.17 µg L(-1), and the relative standard deviation was 2.2% (n=7, c=1 µg L(-1)). The developed method was validated by the analysis of two Certified Reference Materials, and the determined values were in good agreement with the certified values. This method was also successfully applied for the direct analysis of free Cu(II) in human urine and serum samples. While the total Cu can be determined by the proposed method after microwave digestion. The concentrations of free Cu(II) were much lower than that of total Cu, indicating that Cu is mainly coordinated with macromolecules in these biological samples. From this point of view, the developed method exhibits application potential in speciation of free metal ions and metallic complex molecules in biological samples. © 2013 Elsevier B.V. All rights reserved.

  13. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ameli, Akram [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Alizadeh, Naader, E-mail: alizaden@modares.ac.ir [Department of Chemistry, Faculty of Science, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of)

    2011-11-30

    Highlights: Black-Right-Pointing-Pointer Overoxidized polypyrrole templated with salicylate has been utilized as conducting molecular imprinted polymer for EC-SPME. Black-Right-Pointing-Pointer This first study reported on conducting molecular imprinted polymer was used to EC-SPME of salicylate. Black-Right-Pointing-Pointer Proposed method, is particularly effective in sample clean-up and selective monitoring of salicylate in physiological samples. - Abstract: Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5 Multiplication-Sign 10{sup -8} to 5 Multiplication-Sign 10{sup -4} and 1.2 Multiplication-Sign 10{sup -6} to 5 Multiplication-Sign 10{sup -4} mol mL{sup -1} and the detection limit was 4 Multiplication-Sign 10{sup -8} mol L{sup -1}. The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  14. Nonhazardous Urine Pretreatment Method

    Science.gov (United States)

    Akse, James R.; Holtsnider, John T.

    2012-01-01

    A method combines solid phase acidification with two non-toxic biocides to prevent ammonia volatilization and microbial proliferation. The safe, non-oxidizing biocide combination consists of a quaternary amine and a food preservative. This combination has exhibited excellent stabilization of both acidified and unacidified urine. During pretreatment tests, composite urine collected from donors was challenged with a microorganism known to proliferate in urine, and then was processed using the nonhazardous urine pre-treatment method. The challenge microorganisms included Escherichia coli, a common gram-negative bacteria; Enterococcus faecalis, a ureolytic gram-positive bacteria; Candida albicans, a yeast commonly found in urine; and Aspergillus niger, a problematic mold that resists urine pre-treatment. Urine processed in this manner remained microbially stable for over 57 days. Such effective urine stabilization was achieved using non-toxic, non-oxidizing biocides at higher pH (3.6 to 5.8) than previous methods in use or projected for use aboard the International Space Station (ISS). ISS urine pretreatment methods employ strong oxidants including ozone and hexavalent chromium (Cr(VI)), a carcinogenic material, under very acidic conditions (pH = 1.8 to 2.4). The method described here offers a much more benign chemical environment than previous pretreatment methods, and will lower equivalent system mass (ESM) by reducing containment volume and mass, system complexity, and crew time needed to handle pre-treatment chemicals. The biocides, being non-oxidizing, minimize the potential for chemical reactions with urine constituents to produce volatile, airborne contaminants such as cyanogen chloride. Additionally, the biocides are active under significantly less acidic conditions than those used in the current system, thereby reducing the degree of required acidification. A simple flow-through solid phase acidification (SPA) bed is employed to overcome the natural buffering

  15. Traditional Chinese medicine and sports drug testing: identification of natural steroid administration in doping control urine samples resulting from musk (pod) extracts.

    Science.gov (United States)

    Thevis, Mario; Schänzer, Wilhelm; Geyer, Hans; Thieme, Detlef; Grosse, Joachim; Rautenberg, Claudia; Flenker, Ulrich; Beuck, Simon; Thomas, Andreas; Holland, Ruben; Dvorak, Jiri

    2013-01-01

    The administration of musk extract, that is, ingredients obtained by extraction of the liquid secreted from the preputial gland or resulting grains of the male musk deer (eg, Moschus moschiferus), has been recommended in Traditional Chinese Medicine (TCM) applications and was listed in the Japanese pharmacopoeia for various indications requiring cardiovascular stimulation, anti-inflammatory medication or androgenic hormone therapy. Numerous steroidal components including cholesterol, 5α-androstane-3,17-dione, 5β-androstane-3,17-dione, androsterone, etiocholanolone, epiandrosterone, 3β-hydroxy-androst-5-en-17-one, androst-4-ene-3,17-dione and the corresponding urea adduct 3α-ureido-androst-4-en-17-one were characterised as natural ingredients of musk over several decades, implicating an issue concerning doping controls if used for the treatment of elite athletes. In the present study, the impact of musk extract administration on sports drug testing results of five females competing in an international sporting event is reported. In the course of routine doping controls, adverse analytical findings concerning the athletes' steroid profile, corroborated by isotope-ratio mass spectrometry (IRMS) data, were obtained. The athletes' medical advisors admitted the prescription of TCM-based musk pod preparations and provided musk pod samples for comparison purposes to clarify the antidoping rule violation. Steroid profiles, IRMS results, literature data and a musk sample obtained from a living musk deer of a local zoo conclusively demonstrated the use of musk pod extracts in all cases which, however, represented a doping offence as prohibited anabolic-androgenic steroids were administered.

  16. Urine protein electrophoresis test

    Science.gov (United States)

    Urine protein electrophoresis; UPEP; Multiple myeloma - UPEP; Waldenström macroglobulinemia - UPEP; Amyloidosis - UPEP ... special paper and apply an electric current. The proteins move and form visible bands. These reveal the ...

  17. Urinating more at night

    Science.gov (United States)

    ... calcium level Certain medicines, including water pills (diuretics) Diabetes insipidus Waking often during the night to urinate can ... medicines are you taking? Have you changed your diet? Do you drink caffeine and alcohol? If so, ...

  18. Sodium urine test

    Science.gov (United States)

    ... urine sodium level may be a sign of: Adrenal glands releasing too much hormone ( hyperaldosteronism ) Not enough fluid in the body (dehydration) Diarrhea and fluid loss Heart failure Kidney problems, such as chronic kidney disease or ...

  19. PBG urine test

    Science.gov (United States)

    Porphobilinogen test ... temporarily stop taking medicines that may affect the test results. Be sure to tell your provider about ... This test involves only normal urination, and there is no discomfort.

  20. Nanostructured conducting molecularly imprinted polymer for selective extraction of salicylate from urine and serum samples by electrochemically controlled solid-phase micro-extraction.

    Science.gov (United States)

    Ameli, Akram; Alizadeh, Naader

    2011-11-30

    Overoxidized polypyrrole (OPPy) films templated with salicylate (SA) have been utilized as conducting molecular imprinted polymers (CMIPs) for potential-induced selective solid-phase micro-extraction processes. Various important fabrication factors for controlling the performance of the OPPy films have been investigated using fluorescence spectrometry. Several key parameters such as applied potential for uptake, release, pH of uptake and release solution were varied to achieve the optimum micro-extraction procedure. The film template with SA exhibited excellent selectivity over some interference. The calibration graphs were linear in the ranges of 5×10(-8) to 5×10(-4) and 1.2×10(-6) to 5×10(-4)mol mL(-1) and the detection limit was 4×10(-8) mol L(-1). The OPPy film as the solid-phase micro-extraction absorbent has been applied for the selective clean-up and quantification of trace amounts of SA from physiological samples. The results of scanning electron microscopy (SEM) have confirmed the nano-structure morphologies of the films.

  1. USE OF DISPOSABLE DIAPERS TO COLLECT URINE IN EXPOSURE STUDIES

    Science.gov (United States)

    Large studies of children's health as it relates to exposures to chemicals in the environment often require measurements of biomarkers of chemical exposures or effects in urine samples. But collection of urine samples from infants and toddlers is difficult. For large exposure s...

  2. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  3. Day-to-day and within-day variation in urinary iodine excretion

    DEFF Research Database (Denmark)

    Rasmussen, Lone Banke; Ovesen, L.; Christiansen, E.

    1999-01-01

    Objective: To examine the day-to-day and within-day variation in urinary iodine excretion and the day-to-day variation in iodine intake. Design: Collection of consecutive 24-h urine samples and casual urine samples over 24 h. Setting: The study population consisted of highly motivated subjects from...... our Institute. Subjects: Study 1: Ten healthy subjects (seven females and three males) aged 30-46 y. Study 2. Twenty-two healthy subjects (9 males and 13 females) aged 30-55 y. Methods: Study 1: 24-h urine samples were collected for four consecutive days. Study 2. Each urine voided over 24 h...... was collected into separate containers. In both studies dietary records were kept. Main outcome measures: Twenty-four-hour urinary iodine excretion, 24-h urinary iodine excretion estimated as I/Cr*24 h Cr and as a concentration in casual urine samples. Results: Study 1: Both iodine excreted in 24-h urine...

  4. Selective solid-phase extraction of naproxen drug from human urine samples using molecularly imprinted polymer-coated magnetic multi-walled carbon nanotubes prior to its spectrofluorometric determination.

    Science.gov (United States)

    Madrakian, Tayyebeh; Ahmadi, Mazaher; Afkhami, Abbas; Soleimani, Mohammad

    2013-08-21

    A drug imprinted polymer based on suspension polymerization on magnetic multi-walled carbon nanotubes (MIPMCNTs) was prepared with a synthesized amidoamine as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, naproxen (NAP) as the template and ammonium persulfate as the initiator. The MIPMCNTs were characterized by TEM, FT-IR and XRD measurements. The prepared magnetic adsorbent can be well dispersed in aqueous media and can be easily separated magnetically from the medium after loading with NAP. All the aspects influencing the adsorption (extraction time, adsorbent dosage and pH) and desorption (desorption time and desorption solvent) of the analyte on the MIPMCNTs have been investigated. The extracted NAP could be easily desorbed with a mixture of methanol/sodium hydroxide aqueous solution and determined spectrofluorometrically at λem = 353 nm (λex = 271 nm). A linear dynamic range was established from 4.0 to 40.0 ng mL⁻¹ of NAP and the limit of detection (LOD) was found to be 2.0 ng mL⁻¹. In addition, the equilibrium adsorption data of NAP by imprinted polymer were analyzed by Langmuir and Freundlich isotherm models. The developed method was utilized for the determination of NAP in human urine samples with satisfactory results.

  5. Automated extraction of lysergic acid diethylamide (LSD) and N-demethyl-LSD from blood, serum, plasma, and urine samples using the Zymark RapidTrace with LC/MS/MS confirmation.

    Science.gov (United States)

    de Kanel, J; Vickery, W E; Waldner, B; Monahan, R M; Diamond, F X

    1998-05-01

    A forensic procedure for the quantitative confirmation of lysergic acid diethylamide (LSD) and the qualitative confirmation of its metabolite, N-demethyl-LSD, in blood, serum, plasma, and urine samples is presented. The Zymark RapidTrace was used to perform fully automated solid-phase extractions of all specimen types. After extract evaporation, confirmations were performed using liquid chromatography (LC) followed by positive electrospray ionization (ESI+) mass spectrometry/mass spectrometry (MS/MS) without derivatization. Quantitation of LSD was accomplished using LSD-d3 as an internal standard. The limit of quantitation (LOQ) for LSD was 0.05 ng/mL. The limit of detection (LOD) for both LSD and N-demethyl-LSD was 0.025 ng/mL. The recovery of LSD was greater than 95% at levels of 0.1 ng/mL and 2.0 ng/mL. For LSD at 1.0 ng/mL, the within-run and between-run (different day) relative standard deviation (RSD) was 2.2% and 4.4%, respectively.

  6. Screening for human papillomavirus: Is urine useful?

    Directory of Open Access Journals (Sweden)

    D′Hauwers K

    2009-01-01

    Full Text Available Persistent infection with high-risk Human papillomavirus (hr-HPV 16, 18, 31, 33, and 45 is the main risk factor for developing malignant genital lesions. Screening methods and follow-up schedules for cervical cancer are well known. A golden standard to screen and monitor men does not exist yet, because HPV-related, life threatening malignancies in men are rare. The importance of male HPV screening lies mainly in HPV vaccination. Young females are the target group for HPV, but men are considered to be the reservoir for HPV and to have a role in the perpetuation of the infection in the general population. We looked at the usefulness of urine as a tool for HPV screening. Pubmed was searched with the words ′′HPV′′, ′′Urine,′′ and ′′HPV-DNA′′. The chance of finding HPV-DNA in urine is higher in men with lesions in the urethra than outside the urethra, and in women with abnormal cervical cytology. In general, the results of testing urine for HPV-DNA are better for women than for men, probably because of the anatomical position of the urethra to the vagina, vulva, and cervix. In both genders, urine HPV prevalence is higher in HIV pos patients and in high-risk populations. Urine, to screen asymptomatic low-risk-profile (women seems less useful because their urine samples are often inadequate. If urine proves to be the best medium to screen, a low-risk population remains controversial.

  7. Rapid ultrasound-assisted magnetic microextraction of gallic acid from urine, plasma and water samples by HKUST-1-MOF-Fe3O4-GA-MIP-NPs: UV-vis detection and optimization study.

    Science.gov (United States)

    Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

    2017-01-01

    Magnetite (Fe3O4 nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-Fe3O4-GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-Fe3O4-NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV-Vis (UA-DMSPME-UV-Vis) detection method. Plackett-Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-Fe3O4-NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-Fe3O4-NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6mg, 4.0min and 180μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8-6000ngmL(-1) with a Limit of detection (LOD) of 1.377ngmL(-1), limit of quantification (LOQ) 4.591ngmL(-1) and precision (recovery of GA in urine, human plasma and water samples within the range of 92.3-100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application.

  8. Phenylpyruvic acid in urine

    NARCIS (Netherlands)

    Meulemans, O.; Vergeer, E.G.

    1960-01-01

    The method of The, Fleury And Vink for the determination of phenylpyruvic acid (PPA) in urine is modified by measuring the extinction after the green colour with ferric chloride has faded, and subtracting this extinction from that found initially. More accurate values are obtained and low PPA values

  9. Development of an analytical method for the direct determination of uranium isotopes in occupationally exposed personnel urine samples using Icp-SFMS; Desarrollo de un metodo analitico para la determinacion directa de isotopos de uranio en muestras de orina de personal ocupacionalmente expuesto (POE) usando ICP-SFMS

    Energy Technology Data Exchange (ETDEWEB)

    Torres C, C. O.; Hernandez M, H.; Romero G, E. T. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Vega C, H. R., E-mail: hector.hernandez@inin.gob.mx [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98060 Zacatecas, Zac. (Mexico)

    2016-09-15

    The development of an analytical method for measuring actinides in radioactive waste, environmental and biological samples has been a major challenge in institutions dedicated to the nuclear sector. Is for this reason that the developed and validated methods to measure isotopes of elements belonging to the actinide family have as main objective the characterization of radioactive wastes, the monitoring of radioactive installations and the dosimetric evaluation of occupationally exposed personnel, this for the purpose to prevent incidents or radiological accidents and to safeguard workers. This research work is focused on determining isotopes of uranium (U) and obtaining isotope ratios in urine samples of occupationally exposed personnel using a Magnetic Sector Mass Spectrometer with Inductively Coupled Plasma Source (Icp-SFMS), which is a versatile and promising technique for a large number of applications. The urine samples are acidified in order to favor the dissolution of the analytes in the samples, minimizing as much as possible their loss by sorption in the walls of the sampling bottle. For the determination of U in urine samples, dilution was performed, taking 2 ml of the urine samples and weighing it to 100 ml with 2% ultra pure HNO{sub 3} and finally performing the measurement by Icp-SFMS. The results obtained in the measurements of U show an order of magnitude in terms of sensitivity offered by Icp-SFMS. The isotopic ratios {sup 234}U/{sup 238}U, {sup 235}U/{sup 238}U are very close to the results reported by the literature and the quantification of the isotopes of said element show be within the concentration range of U, indicating that is exposed to depleted U. Additionally, Limit of Detection and Quantification Limit calculations were performed, which are of the order of pg mL{sup -1}. (Author)

  10. Genetics Home Reference: maple syrup urine disease

    Science.gov (United States)

    ... links) Genetic Testing Registry: Classical maple syrup urine disease Genetic Testing Registry: Intermediate maple syrup urine disease Genetic Testing Registry: Maple syrup urine disease Other Diagnosis ...

  11. Specificity, sensitivity, and operability of RSID™-urine for forensic identification of urine: comparison with ELISA for Tamm-Horsfall protein.

    Science.gov (United States)

    Akutsu, Tomoko; Watanabe, Ken; Sakurada, Koichi

    2012-11-01

    In this study, the specificity, sensitivity, and operability of RSID™-Urine, a new immunochromatographic test for urine identification, was evaluated and compared with ELISA detection of Tamm-Horsfall protein (THP). Urine was successfully identified among other body fluids using RSID™-Urine and ELISA detection of THP. The detection limit of RSID™-Urine equated to 0.5 μL of urine; although the sensitivity of RSID™-Urine may be lower than that of ELISA detection of THP, it is thought to be sufficient for application to casework samples. However, results from RSID™-Urine must be interpreted with caution when the sample may have been contaminated with blood or vaginal fluid, because this might inhibit urine detection. The RSID™-Urine assay can be performed in just 15 min by dropping the extracted sample onto the test cassette. Therefore, RSID™-Urine should be an effective tool for the forensic identification of urine, in addition to ELISA detection of THP.

  12. Pumping time required to obtain tube well water samples with aquifer characteristic radon concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Ricardo, Carla Pereira; Oliveira, Arno Heeren de, E-mail: heeren@nuclear.ufmg.br [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Escola de Engenharia. Dept. de Engenharia Nuclear; Rocha, Zildete; Palmieri, Helena E.L.; Linhares, Maria G.M.; Menezes, Maria Angela B.C., E-mail: rochaz@cdtn.br, E-mail: help@cdtn.br, E-mail: mgml@cdtn.br, E-mail: menezes@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2011-07-01

    Radon is an inert noble gas, which comes from the natural radioactive decay of uranium and thorium in soil, rock and water. Radon isotopes emanated from radium-bearing grains of a rock or soil are released into the pore space. Radon that reaches the pore space is partitioned between the gaseous and aqueous phases. Thus, the groundwater presents a radon signature from the rock that is characteristic of the aquifer. The characteristic radon concentration of an aquifer, which is mainly related to the emanation, is also influenced by the degree of subsurface degassing, especially in the vicinity of a tube well, where the radon concentration is strongly reduced. Looking for the required pumping time to take a tube well water sample that presents the characteristic radon concentration of the aquifer, an experiment was conducted in an 80 m deep tube well. In this experiment, after twenty-four hours without extraction, water samples were collected periodically, about ten minutes intervals, during two hours of pumping time. The radon concentrations of the samples were determined by using the RAD7 Electronic Radon Detector from Durridge Company, a solid state alpha spectrometric detector. It was realized that the necessary time to reach the maximum radon concentration, that means the characteristic radon concentration of the aquifer, is about sixty minutes. (author)

  13. CHARACTERISTIC OF AIRBORNE PARTICULATE MATTER SAMPLES COLLECTED FROM TWO SEMI INDUSTRIAL SITES IN BANDUNG, INDONESIA

    Directory of Open Access Journals (Sweden)

    Diah Dwiana Lestiani

    2013-12-01

    Full Text Available Air particulate matter concentrations, black carbon as well as elemental concentrations in two semi industrial sites were investigated as a preliminary study for evaluation of air quality in these areas. Sampling of airborne particulate matter was conducted in July 2009 using a Gent stacked filter unit sampler and a total of 18 pairs of samples were collected. Black carbon was determined by reflectance measurement and elemental analysis was performed using particle induced X-ray emission (PIXE. Elements Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, Cr, Mn, Fe, Cu, Zn and As were detected. Twenty four hour PM2.5 concentration at semi industrial sites Kiaracondong and Holis ranged from 4.0 to 22.2 µg m-3, while the PM10 concentration ranged from 24.5 to 77.1 µg m-3. High concentration of crustal elements, sulphur and zinc were identified in fine and coarse fractions for both sites. The fine fraction data from both sites were analyzed using a multivariate principal component analysis and for Kiaracondong site, identified factors are attributed to sea-salt with soil dust, vehicular emissions and biomass burning, non ferrous smelter, and iron/steel work industry, while for Holis site identified factors are attributed to soil dust, industrial emissions, vehicular emissions with biomass burning, and sea-salt. Although particulate samples were collected from semi industrial sites, vehicular emissions constituted with S, Zn and BC were identified in both sites.

  14. Urine Diagnosis for Cancer

    Institute of Scientific and Technical Information of China (English)

    Guo Haiyan; Zhao Baohua

    2002-01-01

    @@ The key to saving the life of a person suffering from a malignant tumor lies in early diagnosis and surgery. Chinese scientists have developed a new method of diagnosing cancer by analyzing a person's urine. This feat was acclaimed by a panel of experts at a meeting under the auspices of the Chinese Academy of Sciences (CAS) in July 30 in Dalian, in northeast China's Liaoning Province.

  15. Towards a method of rapid extraction of strontium-90 from urine: urine pretreatment and alkali metal removal

    Energy Technology Data Exchange (ETDEWEB)

    Hawkins, C. [Argonne National Lab. (ANL), Argonne, IL (United States); Dietz, M. [Argonne National Lab. (ANL), Argonne, IL (United States); Kaminski, M. [Argonne National Lab. (ANL), Argonne, IL (United States); Mertz, C. [Argonne National Lab. (ANL), Argonne, IL (United States); Shkrob, I. [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-03-01

    A technical program to support the Centers of Disease Control and Prevention is being developed to provide an analytical method for rapid extraction of Sr-90 from urine, with the intent of assessing the general population’s exposure during an emergency response to a radiological terrorist event. Results are presented on the progress in urine sample preparation and chemical separation steps that provide an accurate and quantitative detection of Sr-90 based upon an automated column separation sequence and a liquid scintillation assay. Batch extractions were used to evaluate the urine pretreatment and the column separation efficiency and loading capacity based upon commercial, extractant-loaded resins. An efficient pretreatment process for decolorizing and removing organics from urine without measurable loss of radiostrontium from the sample was demonstrated. In addition, the Diphonix® resin shows promise for the removal of high concentrations of common strontium interferents in urine as a first separation step for Sr-90 analysis.

  16. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples. II. Determination of clenbuterol in urine using multiple-stage mass spectrometry in an ion-trap mass spectrometer

    NARCIS (Netherlands)

    van Hout, MWJ; Hofland, CM; Niederlander, HAG; de Jong, GJ

    2000-01-01

    Solid-phase extraction (SPE) was coupled to ion-trap mass spectrometry to determine clenbuterol in urine. For SPE a cartridge exchanger was used and, after extraction, the eluate was directly introduced into the mass spectrometer, For two types of cartridges, i.e. C-18 and polydivinylbenzene (PDVB),

  17. Selenium speciation in pretreated human urine by ion-exchange chromatography and ICP-MS detection

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.; Bendahl, L.

    2001-01-01

    Urine samples were extracted by benzo-15-crown-5-ether to remove sodium and potassium. More than 90% of the sodium and potassium content of the urine was removed with this extraction. In a cation-exchange system based on oxalic acid at pH 3, chromatography of an untreated urine pool resulted in a...

  18. Avian bornavirus in the urine of infected birds

    Directory of Open Access Journals (Sweden)

    Villalobos AR

    2012-06-01

    Full Text Available J Jill Heatley,1 Alice R Villalobos21Zoological Medicine, 2Department of Nutrition & Food Science, Texas A&M University, College of Veterinary Medicine and Biomedical Sciences, College Station, TX, USAAbstract: Avian bornavirus (ABV causes proventricular dilatation disease in multiple avian species. In severe clinical disease, the virus, while primarily neurotropic, can be detected in many organs, including the kidneys. We postulated that ABV could be shed by the kidneys and found in the urine of infected birds. Immunohistochemical staining demonstrated viral N and P proteins of ABV within the renal tubules. We adapted a nonsurgical method of urine collection for use in parrots known to be shedding ABV in their droppings. We obtained urine without feces, and results were compared with swabs of fresh voided feces. Reverse transcription–polymerase chain reaction assay performed on these paired samples from five birds indicated that ABV was shed in quantity in the urine of infected birds, and a single sample was urine-positive and fecal-negative. We suggest that urine sampling may be a superior sample for detection of birds shedding ABV, and advocate that additional birds, known to be shedding or infected with ABV, should be investigated via this method.Keywords: avian bornavirus, Psittaciformes, parrot, urine, proventricular dilatation disease

  19. Measurement of Orotic Acid in Urine by Supercritical Fluid Chromatography

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    This work presents a simple, rapid and reliable supercritical fluid chromatography (SFC) method for a sensitive measurement of orotic acid in human urine. The samples were diluted with deionized water and analyzed directly without any pretreatment.

  20. Studies related to the origin of C18 neutral steroids isolated from extracts of urine from the male horse: the identification of urinary 19-oic acids and their decarboxylation to produce estr-4-en-17beta-ol-3-one (19-nortestosterone) and estr-4-ene-3,17-dione (19-norandrost-4-ene-3,17-dione) during sample processing.

    Science.gov (United States)

    Houghton, E; Teale, P; Dumasia, M C

    2007-03-14

    For almost two decades we have known that enzymatic hydrolysis of "normal" urine samples from the entire male horse using Escherichia coli (E. coli) followed by solvolysis (ethyl acetate:methanol:sulphuric acid) results in the detection of significant amounts of estr-4-ene-3,17-dione (19-norandrost-4-ene-3,17-dione) along with estr-4-en-17beta-ol-3-one (19-nortestosterone, nandrolone) in extracts of the hydrolysed urine and that both steroids are isolated from the solvolysis fraction. This solvolysis process is targeted at the steroid sulphates. Also we have shown that 19-norandrost-4-ene-3,17-dione and 19-nortestosterone are isolated from testicular tissue extracts. Subsequently, evidence was obtained that 19-nortestosterone detected in extracts of "normal" urine from male horses may not be derived from the 17beta-sulphate conjugate. However, following administration of 19-nortestosterone based proprietary anabolic steroids to all horses (males, females and castrates), the urinary 19-nortestosterone arising from the administration is excreted primarily as the 17beta-sulphate conjugate. Thus, if the 19-nortestosterone-17beta-sulphate conjugate arises only following administration this has interesting implications for drug surveillance programmes to control administration of 19-nortestosterone based anabolic preparations to male horses. These results have led us to consider that the precursors to 19-nortestosterone and 19-norandrost-4-ene-3,17-dione, present in the urine prior to the hydrolysis steps, have the same basic structure except for the functionality at the 17-position. We have used preparative high pressure liquid chromatography (LC) and LC fractionation to separate these precursors from the high amounts of oestrogenic sulphates present in "normal" urine from the entire male horse. Purified fractions have then been studied by liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) to identify the precursors.

  1. Adulterants in Urine Drug Testing.

    Science.gov (United States)

    Fu, S

    Urine drug testing plays an important role in monitoring licit and illicit drug use for both medico-legal and clinical purposes. One of the major challenges of urine drug testing is adulteration, a practice involving manipulation of a urine specimen with chemical adulterants to produce a false negative test result. This problem is compounded by the number of easily obtained chemicals that can effectively adulterate a urine specimen. Common adulterants include some household chemicals such as hypochlorite bleach, laundry detergent, table salt, and toilet bowl cleaner and many commercial products such as UrinAid (glutaraldehyde), Stealth® (containing peroxidase and peroxide), Urine Luck (pyridinium chlorochromate, PCC), and Klear® (potassium nitrite) available through the Internet. These adulterants can invalidate a screening test result, a confirmatory test result, or both. To counteract urine adulteration, drug testing laboratories have developed a number of analytical methods to detect adulterants in a urine specimen. While these methods are useful in detecting urine adulteration when such activities are suspected, they do not reveal what types of drugs are being concealed. This is particularly the case when oxidizing urine adulterants are involved as these oxidants are capable of destroying drugs and their metabolites in urine, rendering the drug analytes undetectable by any testing technology. One promising approach to address this current limitation has been the use of unique oxidation products formed from reaction of drug analytes with oxidizing adulterants as markers for monitoring drug misuse and urine adulteration. This novel approach will ultimately improve the effectiveness of the current urine drug testing programs. © 2016 Elsevier Inc. All rights reserved.

  2. Application of electrolysis for detoxification of an antineoplastic in urine.

    Science.gov (United States)

    Kobayashi, Toyohide; Hirose, Jun; Sano, Kouichi; Kato, Ryuji; Ijiri, Yoshio; Takiuchi, Hiroya; Tanaka, Kazuhiko; Goto, Emi; Tamai, Hiroshi; Nakano, Takashi

    2012-04-01

    Antineoplastics in excreta from patients have been considered to be one of the origins of cytotoxic, carcinogenic, teratogenic, and mutagenic contaminants in surface water. Recent studies have demonstrated that antineoplastics in clinical wastewater can be detoxified by electrolysis. In this study, to develop a method for the detoxification of antineoplastics in excreta, methotrexate solution in the presence of human urine was electrolyzed and evaluated. We found that urine inhibits detoxification by electrolysis; however, this inhibition decreased by diluting urine. In urine samples, the concentrations of active chlorine generated by anodic oxidation from 0.9% NaCl solution for inactivation of antineoplastics increased in dilution-dependent and time-dependent manner. These results indicate that electrolysis with platinum-based iridium oxide composite electrode is a possible method for the detoxification of a certain antineoplastic in urine.

  3. Hybrid molecularly imprinted polymers synthesized with 3-aminopropyltriethoxysilane-methacrylic acid monomer for miniaturized solid-phase extraction: A new and economical sample preparation strategy for determination of acyclovir in urine.

    Science.gov (United States)

    Yan, Hongyuan; Wang, Mingyu; Han, Yehong; Qiao, Fengxia; Row, Kyung Ho

    2014-06-13

    The miniaturized molecularly imprinted solid-phase extraction (mini-MISPE) coupled with high-performance liquid chromatography was proposed for the determination of acyclovir in urine. 1.5-mL tapered plastic centrifuge tube filled with hybrid molecularly imprinted polymers (HMIPs) was used as the cartridge of mini-MISPE, and the HMIPs synthesized with 3-aminopropyltriethoxy silane-methacrylic acid as monomer exhibited good recognition and selectivity for acyclovir. Under the optimized condition, good linear calibration was obtained in a range of 0.5-15μgmL(-1) with the correlation coefficient of 0.9994, and the recoveries at three spiked levels were 91.6-103.3% in urine with the relative standard deviation (RSD) of ≤3.5%. Excellent intra-day and inter-day repeatability were achieved with RSD of ≤2.6% and 4.0% in three different concentrations. This method combined the advantages of HMIPs and mini-MISPE, and it could become an alternative tool for analyzing the residues of acyclovir in complex urine matrices.

  4. Profiles of phytoestrogens in human urine from several Asian countries.

    Science.gov (United States)

    Kunisue, Tatsuya; Tanabe, Shinsuke; Isobe, Tomohiko; Aldous, Kenneth M; Kannan, Kurunthachalam

    2010-09-08

    Intake of a diet rich in phytoestrogens has been associated with a decreased risk for hormone-dependent cancers in humans. Biomonitoring of phytoestrogens in human urine has been used to assess the intake of phytoestrogens. Although studies have reported phytoestrogen levels in urine specimens from the United States and Japan, little is known of human intake of phytoestrogens in other Asian countries. In this study we determined the concentrations of seven phytoestrogens, namely, enterolactone, enterodiol, daidzein, equol, O-desmethylangolensin (O-DMA), genistein, and coumestrol, in 199 human urine samples from three Asian countries, Vietnam (Hanoi and Ho Chi Minh), Cambodia (Phnom Penh), and India (Chennai and Kolkata), using a simple, sensitive, and reliable liquid chromatography (LC)-tandem mass spectrometry (MS/MS) method. The residue levels of phytoestrogens in urine samples from the three Asian countries were compared with the concentrations in 26 urine samples from Japan (Ehime) and 16 urine samples from the United States (Albany), analyzed in this study. Among the phytoestrogens analyzed, isoflavones such as daidzein and genistein were predominant in urine samples from Vietnam; samples from Cambodia and India contained higher concentrations of enterolactone than isoflavones. Urinary concentrations of isoflavones in samples from Hanoi, Vietnam, were notably higher than the concentrations in samples from Cambodia, India, and the United States and similar to the concentrations in samples from Japan. The lowest concentrations of daidzein and the highest concentrations of enterolactone were found in urine samples from India. Concentrations of equol and O-DMA, which are microbial transformation products of daidzein (produced by gut microflora), were notably high in urine samples from Hanoi, Vietnam. The ratios of the concentration of equol or O-DMA to that of daidzein were significantly higher in samples from Hanoi than from Japan, indicating high

  5. Assessment Of NPK In Human Male And Female Urine For Its Fertilising Potential In Agriculture

    Directory of Open Access Journals (Sweden)

    Alfred L.K. Kuwornu

    2015-08-01

    Full Text Available ABSTRACT The study evaluated concentrations of Nitrogen Phosphorus and Potassium in male and female urine stored over six months and its potential as a fertilizing agent in agriculture. Urinals were constructed to allow for easy collection of male and female urine and then stored in transparent bottles for six months in a greenhouse. Monthly triplicate analysis of male and female urine was done for nitrogen phosphorus potassium temperature pH and colour change. Bray P1 and Flame photometry methods were used in the determination of phosphorus and potassium contents and Kjedahl digestion and non-digestion direct methods for nitrogen content. Temperature pH and colour were determined using mercury thermometer temperaturepH meter and a colour chart. Results showed that nitrogen in female urine was significantly p0.05 higher than that in male urine after 2 to 5 months of storage. However there were no significant differences p0.05 with respect to the direct method. Contrastingly phosphorus in male urine was significantly p0.05 higher than that in female urine after 2 to 3 months of storage but there were no significant differences in potassium content for all male and female urine samples. Generally NPK yields in both urine sources peaked four months after storage. There was a moderate positive correlation between the direct female urine Nitrogen and storage time. The phosphorus levels also correlated positively with storage time and temperature but weakly negative with pH. Generally urine nitrogen strongly correlated positively with potassium but moderately with temperature and pH. Colour of matured urine after six months storage was yellow for females and brown for males. NPK contents in both male 30.43.4-1-43.7 and female 34.46.5-1-62.8 urine were comparable to those of chemical fertilizers such as 21 N ammonia. However the nitrogen content of digested female urine was significantly higher than that of male urine. Phosphorus concentration was

  6. 24小时食管多通道腔内阻抗联合pH监测技术在早产儿中的应用%Role of the twenty-four-hour esophageal multichannel intraluminal impedance-pH monitoring in preterm infants

    Institute of Scientific and Technical Information of China (English)

    张娟; 李在玲; 葛颖; 王琨; 徐志杰; 夏至伟; 段丽萍

    2014-01-01

    Objective To evaluate the clinical application of 24-hour esophageal muhichannel intraluminal impedance-pH monitoring technique in preterm infants.Method This study enrolled 28 preterm(male 20,female 8)infants with symptoms suggestive of gastroesophageal reflux (GER) (frequent regurgitations,apnea,or transcutaneous oxygen saturation decreased).They had postmenstrual age from 26 to 32 weeks,median (28.9 ± 1.9) weeks,had birth weight from 850 to 1 700 g,median (1 250.4 ±272.8)g,range 850-1700 g,and were studied at corrected gestational age from 28 to 40 weeks,median (34.5 ± 2.3) weeks.Combined measurement of esophageal pH and impedance was performed.The 24-hour pH-impedance recording was uploaded onto a portable storage card and for computer-assisted manual analysis,using a specialized software program.When values were distributed normally,they were presented as mean and standard deviation,compared using t test.When values were not distributed normally,they were presented as median,minimum and maximum.Median values were compared using the Mann-Whitney U non-parametric test.SPSS 17.0 software was used.Result In 28 preterm infants,71.4% (20/28) had pathological acid refluxes with pH monitor,while 100% with combined measurement of esophageal pH and impedance.Gestational age,birth weight,corrected gestational age had no association with acid GER.Frequent regurgitations,apnea,or transcutaneous oxygen saturation decreased but there was no statistically significant difference between acid GER group and non-acid GER group.Eight cases had no pathological acid refluxes,but showed an increase of weakly acid refluxes than pathological acid refluxes group (P <0.01).The median number of reflux events in 24 hours for 28 cases was 64.5 (0-377),23.4% were acidic,while 76.4% were weakly acidic; 59.1% were liquid bolus refluxes,while 40.9% were mixed bolus refluxes.The positive ratio of symptoms related index and symptoms association probability were significantly increased combined measurement of esophageal pH and impedance versus pH monitor were used.Conclusion The 24-hour esophageal impedance-pH monitoring technique was safe and had good tolerance.We confirmed that it detected more weakly acidic refluxes,liquid bolus refluxes,and mixed bolus refluxes.And it provided more evidence for explaining the relationship between GER and clinical manifestation.%目的 评价24 h食管多通道腔内阻抗(MⅡ)联合pH监测技术在早产儿中的临床应用情况.方法 28例临床考虑有胃食管反流(GER)症状(呕吐、呼吸暂停、氧饱和度下降)的早产儿.其中男20例,女8例,胎龄26 ~ 32周,平均(28.9±1.9)周,出生体重850 ~1 700 g,平均(1 250.4±272.8)g,检查时矫正胎龄28 ~40周,平均(34.5±2.3)周.行24 h食管MⅡ及pH监测,数据被保存在便携式记录器的储存卡内用专业软件分析.将传统pH值监测指标阳性患儿归为GER阳性组,阴性为GER阴性组.采用SPSS 17.0软件,计量资料呈正态分布的以均数±标准差表示,采用t检验;非正态分布的用中位数(范围)表示,采用Mann-Whitney U非参数检验.结果 28例早产儿中,pH值监测法GER检出率为71.4%(20/28),MⅡ联合pH值法检出率为100%,优于pH值检测法.胎龄、出生体重、矫正胎龄与GER无关.氧饱和度下降、呼吸暂停、呕吐症状在GER阳性组及GER阴性组间差异无统计学意义.8例GER阴性组无病理性酸反流,但阻抗监测提示弱酸反流较GER阳性组增加(P<0.01).28例患儿24h总反流事件中位数为64.5(0~377)次,其中酸反流占总反流事件的23.4%,弱酸反流占所有反流事件的76.4%.液体反流占总反流的59.1%,混合反流占总反流40.9%.MⅡ联合pH监测使症状相关指数和症状联合概率阳性比率较应用pH监测时明显升高.结论 24 h MⅡ联合pH监测技术应用于早产儿安全性高,具有较好的耐受性.可发现弱酸反流及液体、混合反流,为更好地解释GER与临床表现的关系提供了可能.

  7. Toward a standardized urine proteome analysis methodology.

    Science.gov (United States)

    Court, Magali; Selevsek, Nathalie; Matondo, Mariette; Allory, Yves; Garin, Jerome; Masselon, Christophe D; Domon, Bruno

    2011-03-01

    Urine is an easily accessible bodily fluid particularly suited for the routine clinical analysis of disease biomarkers. Actually, the urinary proteome is more diverse than anticipated a decade ago. Hence, significant analytical and practical issues of urine proteomics such as sample collection and preparation have emerged, in particular for large-scale studies. We have undertaken a systematic study to define standardized and integrated analytical protocols for a biomarker development pipeline, employing two LC-MS analytical platforms, namely accurate mass and time tags and selected reaction monitoring, for the discovery and verification phase, respectively. Urine samples collected from hospital patients were processed using four different protocols, which were evaluated and compared on both analytical platforms. Addition of internal standards at various stages of sample processing allowed the estimation of protein extraction yields and the absolute quantification of selected urinary proteins. Reproducibility of the entire process and dynamic range of quantification were also evaluated. Organic solvent precipitation followed by in-solution digestion provided the best performances and was thus selected as the standard method common to the discovery and verification phases. Finally, we applied this protocol for platforms' cross-validation and obtained excellent consistency between urinary protein concentration estimates by both analytical methods performed in parallel in two laboratories. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Cortisol in urine and saliva

    DEFF Research Database (Denmark)

    Hurwitz Eller, N; Netterstrøm, B; Hansen, Åse Marie

    2001-01-01

    The objective of the study was to analyse the relations between excretion of cortisol in urine and saliva and the intima media thickness (IMT) of the artery carotis communis.......The objective of the study was to analyse the relations between excretion of cortisol in urine and saliva and the intima media thickness (IMT) of the artery carotis communis....

  9. Prevalence of isolated non-albumin proteinuria in the US population tested for both, urine total protein and urine albumin: An unexpected discovery.

    Science.gov (United States)

    Katayev, Alexander; Zebelman, Arthur M; Sharp, Thomas M; Samantha Flynn; Bernstein, Richard K

    2017-04-01

    Isolated non-albumin proteinuria (NAP) is a condition when urine total protein concentrations are elevated without elevation of urine albumin. The prevalence of NAP in the US population tested for both, urine total protein and albumin was assessed in this study. The database of a US nationwide laboratory network was queried for test results when random urine albumin was ordered together with urine total protein and also when timed 24-hour urine albumin was ordered together with urine total protein. The total prevalence of NAP in the US population tested for both, urine total protein and albumin was calculated for patient groups having normal and low-normal urine albumin (random and timed) with elevated and severely increased urine total protein (random and timed). Also, the prevalence of NAP was calculated for patients with normal urine albumin to assess the probability of missing proteinuria if only urine albumin is measured. The prevalence of NAP in the random samples group was 10.1% (15.2% for females and 4.7% for males). Among patients with normal random albumin, there were 20.0% (27.3% of females and 10.7% of males) patients with NAP. The prevalence of NAP in the timed samples group was 24.6% (29.8% for females and 18.5% for males). Among patients with normal timed urine albumin, there were 36.2% (40.0% of females and 30.8% of males) patients with NAP. There was a strong positive association with female gender and NAP in most patients groups. Testing for only urine (micro)albumin can miss up to 40% of females and 30.8% of males with gross proteinuria. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  10. [Pastel in the urine bag].

    Science.gov (United States)

    Cantaloube, Lucie; Lebaudy, Cécile; Hermabessière, Sophie; Rolland, Yves

    2012-03-01

    Purple urine bag syndrome is a relatively unknown phenomenon in which the urine bag and the collector of chronically catheterized patients turn purple or blue. It affects predominantly women, and is mainly reported in elderly patients. The mechanism seems to be related to the appearance in the urine of two compounds that have been identified as indigo (blue) and indirubin (red) which bind to the urine bag and the collector. Several associated factors are usually mentioned such as constipation, alkaline urine, bed rest, institutionalization or cognitive impairment. They are risk factor of this phenomenon. On the other hand, an infection or a urinary bacterial colonization is necessary and high bacterial counts seem to be the critical step in the development of the purple urine bag syndrome. We report on two cases of purple urine bag syndrome observed in two patients being treated in a long-term care unit. Both of whom were diagnosed with indwelling urinary bacterial colonization, with Escherichia coli and Pseudomonas aeruginosa respectively.

  11. Estimate of dietary phosphorus intake using 24-h urine collection.

    Science.gov (United States)

    Morimoto, Yuuka; Sakuma, Masae; Ohta, Hiroyuki; Suzuki, Akitsu; Matsushita, Asami; Umeda, Minako; Ishikawa, Makoto; Taketani, Yutaka; Takeda, Eiji; Arai, Hidekazu

    2014-07-01

    Increases in serum phosphorus levels and dietary phosphorus intake induces vascular calcification, arterial sclerosis and cardiovascular diseases. Limiting phosphorus intake is advisable, however, no assessment methods are capable of estimating dietary phosphorus intake. We hypothesized that urinary phosphorus excretion can be translated into estimation of dietary phosphorus intake, and we evaluated whether a 24-h urine collection method could estimate dietary phosphorus intake. Thirty two healthy subjects were recruited for this study. Subjects collected urine samples over 24 h and weighed dietary records. We calculated dietary protein intake and phosphorus intake from dietary records and urine collection, and investigated associations between the two methods in estimating protein and phosphorus intake. Significant positive correlations were observed between dietary records and UC for protein and phosphorus intake. The average intakes determined from dietary records were significantly higher than from urine collection for both protein and phosphorus. There was a significant positive correlation between both the phosphorus and protein difference in dietary records and urine collection. The phosphorus-protein ratio in urine collection was significantly higher than in dietary records. Our data indicated that the 24-h urine collection method can estimate the amount of dietary phosphorus intake, and the results were superior to estimation by weighed dietary record.

  12. Urine sediment from a Chihuahua.

    Science.gov (United States)

    Pallatto, Valarie; Wood, Michael; Grindem, Carol

    2005-12-01

    A 6-year-old, intact male Chihuahua was presented with stranguria and painful urination of 5 days duration. Cystine crystals were observed in low numbers in unstained urine sediment preparations, and a diagnosis of cystinuria was made. Uroliths were removed surgically from the urethra and the bladder, and mineral analysis indicated the stones were composed of 100% cystine. Cystinuria results from an inherited defect in renal tubular transport of cystine that affects many breeds and has been found as an autosomal recessive trait in Newfoundlands. Accurate identification of cystine crystals in urine is an important means of diagnosing cystinuria.

  13. Mining the human urine proteome for monitoring renal transplant injury

    Energy Technology Data Exchange (ETDEWEB)

    Sigdel, Tara K.; Gao, Yuqian; He, Jintang; Wang, Anyou; Nicora, Carrie D.; Fillmore, Thomas L.; Shi, Tujin; Webb-Robertson, Bobbie-Jo; Smith, Richard D.; Qian, Wei-Jun; Salvatierra, Oscar; Camp, David G.; Sarwal, Minnie M.

    2016-06-01

    The human urinary proteome reflects systemic and inherent renal injury perturbations and can be analyzed to harness specific biomarkers for different kidney transplant injury states. 396 unique urine samples were collected contemporaneously with an allograft biopsy from 396 unique kidney transplant recipients. Centralized, blinded histology on the graft was used to classify matched urine samples into categories of acute rejection (AR), chronic allograft nephropathy (CAN), BK virus nephritis (BKVN), and stable graft (STA). Liquid chromatography–mass spectrometry (LC-MS) based proteomics using iTRAQ based discovery (n=108) and global label-free LC-MS analyses of individual samples (n=137) for quantitative proteome assessment were used in the discovery step. Selected reaction monitoring (SRM) was applied to identify and validate minimal urine protein/peptide biomarkers to accurately segregate organ injury causation and pathology on unique urine samples (n=151). A total of 958 proteins were initially quantified by iTRAQ, 87% of which were also identified among 1574 urine proteins detected in LC-MS validation. 103 urine proteins were significantly (p<0.05) perturbed in injury and enriched for humoral immunity, complement activation, and lymphocyte trafficking. A set of 131 peptides corresponding to 78 proteins were assessed by SRM for their significance in an independent sample cohort. A minimal set of 35 peptides mapping to 33 proteins, were modeled to segregate different injury groups (AUC =93% for AR, 99% for CAN, 83% for BKVN). Urinary proteome discovery and targeted validation identified urine protein fingerprints for non-invasive differentiation of kidney transplant injuries, thus opening the door for personalized immune risk assessment and therapy.

  14. Diagnosis of neonatal group B Streptococcus sepsis by nested-PCR of residual urine samples Diagnóstico de sepse neonatal causada pelo estreptococo do grupo B por meio de dupla amplificação de amostras residuais de urina

    Directory of Open Access Journals (Sweden)

    Bruno Nicolino Cezarino

    2008-03-01

    Full Text Available Group B streptococcus (GBS remains the most common cause of early-onset sepsis in newborns. Laboratory gold-standard, broth culture methods are highly specific, but lack sensitivity. The aim of this study was to validate a nested-PCR and to determine whether residue volumes of urine samples obtained by non invasive, non sterile methods could be used to confirm neonatal GBS sepsis. The nested-PCR was performed with primers of the major GBS surface antigen. Unavailability of biological samples to perform life supporting exams, as well as others to elucidate the etiology of infections is a frequent problem concerning newborn patients. Nevertheless, we decided to include cases according to strict criteria: newborns had to present with signs and symptoms compatible with GBS infection; at least one of the following biological samples had to be sent for culture: blood, urine, or cerebrospinal fluid; availability of residue volumes of the samples sent for cultures, or of others collected on the day of hospitalization, prior to antibiotic therapy prescription, to be analyzed by PCR; favorable outcome after GBS empiric treatment. In only one newborn GBS infection was confirmed by cultures, while infection was only presumptive in the other three patients (they fulfilled inclusion criteria but were GBS-culture negative. From a total of 12 biological samples (5 blood, 3 CSF and 4 urine specimen, eight were tested by culture methods (2/8 were positive, and 8 were tested by PCR (7/8 were positive, and only 4 samples were simultaneously tested by both methods (1 positive by culture and 3 by PCR. In conclusion, although based on a restricted number of neonates and samples, our results suggest that the proposed nested-PCR might be used to diagnose GBS sepsis as it has successfully amplified the three types of biological samples analyzed (blood, urine and cerebrospinal fluid, and was more sensitive than culture methods as PCR in urine confirmed diagnosis in all

  15. An emergency bioassay method for (210)Po in urine.

    Science.gov (United States)

    Guérin, Nicolas; Dai, Xiongxin

    2015-09-01

    A rapid method was developed to efficiently measure (210)Po in urine samples in an emergency situation. Polonium-210 in small urine samples (10 mL) was spontaneously deposited on a stainless steel disc in 1 M HCl at room temperature for 4 h in a polyethylene bottle. The metallic disc was then counted for 4 h by alpha spectrometry. The developed method allowed the preparation of large sample batch in a short time. The method meets the requirements for an emergency bioassay procedure.

  16. Rheological and Infrared Spectroscopic Investigations of Normal and Chronic Kidney Disease Urine

    Directory of Open Access Journals (Sweden)

    Syed Ismail Ahmad

    2016-06-01

    Full Text Available The objective of the study is to examine the physical properties of urine of healthy donors and Chronic Kidney Disease (CKD patients for possible early detection of proteinuria. Specific gravity, viscosity, surface tension, refractive index, electrical conductivity and IR spectroscopy of urine were studied. First morning urine and random urine samples were collected from healthy male donors and were considered as controls to compare with CKD patients. Urine from healthy donors treated with albumin also used in the study. The decrease in surface tension of CKD urines was observed due to high albumin excretion and increased blood urea nitrogen. Fourier Transform Infrared (FTIR spectra in the mid IR region were recorded for normal and albumin treated urine. It observed that peaks at 1641 cm-1 and 1450 cm-1 in IR spectra are the most specific peaks for urea and albumin, respectively. This method of detecting proteinuria is quick and cheaper, and is an alternate to eGFR.

  17. Treating urine by Spirulina platensis

    Science.gov (United States)

    Yang, Chenliang; Liu, Hong; Li, Ming; Yu, Chengying; Yu, Gurevich

    In this paper Spirulina platensis with relatively high nutrition was cultivated to treat human urine. Batch culture showed that the consumption of N in human urine could reach to 99%, and the consumption of P was more than 99.9%, and 1.05 g biomass was obtained by treating 12.5 ml synthetic human urine; continuous culture showed that S. platensis could consume N, Cl, K and S in human urine effectively, and the consumption could reach to 99.9%, 75.0%, 83.7% and 96.0%, respectively, and the consumption of P was over 99.9%, which is very important to increase the closure and safety of the bioregenerative life support system (BLSS).

  18. Urine antigen detection for the diagnosis of human neurocysticercosis.

    Science.gov (United States)

    Castillo, Yesenia; Rodriguez, Silvia; García, Hector H; Brandt, Jef; Van Hul, Anke; Silva, Maria; Rodriguez-Hidalgo, Richar; Portocarrero, Mylagritos; Melendez, D Paolo; Gonzalez, Armando E; Gilman, Robert H; Dorny, Pierre

    2009-03-01

    Neurocysticercosis (NCC) is a major cause of seizures and epilepsy. Diagnosis is based on brain imaging, supported by immunodiagnosis in serum or cerebrospinal fluid (CSF). Lumbar puncture is invasive and painful. Blood sampling is slightly painful and poorly accepted. Urine antigen detection has been used for other parasites and tried in NCC with suboptimal performance. We used a monoclonal antibody-based ELISA to detect Taenia solium antigens in urine from 87 Peruvian neurocysticercosis patients (viable cysts, N = 34; subarachnoid cysticercosis, N = 10; degenerating parasites, N = 7; calcified lesions, N = 36) and 32 volunteers from a non-endemic area of Peru. Overall sensitivity of urine antigen detection for viable parasites was 92%, which decreased to 62.5% in patients with a single cyst. Most patients (30/36, 83%) with only calcified cysticercosis were urine antigen negative. Antigen levels in paired serum/urine samples (evaluated in 19 patients) were strongly correlated. Non-invasive urine testing for T. solium antigens provides a useful alternative for NCC diagnosis.

  19. Quantification of hepatic carbohydrate metabolism in conscious mice using serial blood and urine spots

    NARCIS (Netherlands)

    van Dijk, TH; Boer, TS; Havinga, R; Stellaard, F; Kuipers, F; Reijngoud, DJ

    2003-01-01

    In vivo studies of hepatic carbohydrate metabolism in (genetically modified) conscious mice are hampered by limitations of blood and urine sample sizes. We developed and validated methods to quantify stable isotope dilution and incorporation in small blood and urine samples spotted onto filter paper

  20. Quantification of hepatic carbohydrate metabolism in conscious mice using serial blood and urine spots

    NARCIS (Netherlands)

    van Dijk, TH; Boer, TS; Havinga, R; Stellaard, F; Kuipers, F; Reijngoud, DJ

    2003-01-01

    In vivo studies of hepatic carbohydrate metabolism in (genetically modified) conscious mice are hampered by limitations of blood and urine sample sizes. We developed and validated methods to quantify stable isotope dilution and incorporation in small blood and urine samples spotted onto filter

  1. Urine proteomic profiling of uranium nephrotoxicity

    Energy Technology Data Exchange (ETDEWEB)

    Malard, V.; Gaillard, J.C.; Sage, N. [CEA, DSV, IBEB, SBTN, Laboratoire de Biochimie des Systemes Perturbes (LBSP), Bagnols-sur-Ceze, F-30207 (France); Berenguer, F. [CEA, DSV, IBEB, SBTN, Laboratoire d' Etude des Proteines Cibles (LEPC), Bagnols-sur-Ceze, F-30207 (France); Quemeneur, E. [CEA, DSV, IBEB, SBTN, Bagnols-sur-Ceze, F-30207 (France)

    2009-07-01

    Uranium is used in many chemical forms in civilian and military industries and is a known nephro-toxicant. A key issue in monitoring occupational exposure is to be able to evaluate the potential damage to the body, particularly the kidney. In this study we used innovative proteomic techniques to analyse urinary protein modulation associated with acute uranium exposure in rats. Given that the rat urinary proteome has rarely been studied, we first identified 102 different proteins in normal urine, expanding the current proteome data set for this central animal in toxicology. Rats were exposed intravenously to uranyl nitrate at 2.5 and 5 mg/kg and samples were collected 24 h later. Using two complementary proteomic methods, a classic 2-DE approach and semi-quantitative SDS-PAGE-LC-MS/MS, 14 modulated proteins (7 with increased levels and 7 with decreased levels) were identified in urine after uranium exposure. Modulation of three of them was confirmed by western blot. Some of the modulated proteins corresponded to proteins already described in case of nephrotoxicity, and indicated a loss of glomerular permeability (albumin, alpha-1-anti-proteinase, sero-transferrin). Others revealed tubular damage, such as EGF and vitamin D-binding protein. A third category included proteins never described in urine as being associated with metal stress, such as ceruloplasmin. Urinary proteomics is thus a valuable tool to profile uranium toxicity non-invasively and could be very useful in follow-up in case of accidental exposure to uranium. (authors)

  2. Psychopathology and urine toxicology in methadone patients

    Directory of Open Access Journals (Sweden)

    Gamal Sadek

    2015-06-01

    Full Text Available Several studies reported high rates of psychiatric commorbidity among methadone patients. We examined the relationships of measures of psychopathology to outcomes of screening urine tests for cocaine, opiates, and benzodiazepines in a sample of 56 methadone patients. They also completed the Symptom Check List-90-Revised (SCL-90-R. The highest scales in the SCL-90-R profile of our patients were those indicating somatic discomfort, anger, phobic anxiety, paranoid ideation, and also obsessive-compulsive disorder symptoms (scores above the 39th percentile. The only significant correlations between urine tests and SCL-90-R psychopathology were those involving benzodiazepines: patients with urine tests positive for benzodiazepines had lower social self-confidence (r=0.48, were more obsessive-compulsive (r=0.44, reported a higher level of anger (r=0.41, of phobic tendencies (r=40, of anxiety (r=0.39, and of paranoid tendencies (r=0.38, and also reported more frequent psychotic symptoms (r=0.43.

  3. Antibiotic Screening of Urine Culture for Internal Quality Audit at Amrita Hospital, Kochi.

    Science.gov (United States)

    Suresh, Aswathy; Gopinathan, Anusha; Dinesh, Kavitha R; Kumar, Anil

    2017-07-01

    Urine antimicrobial activity is a seldom analysed laboratory test which greatly impacts the quantification of urine specimens. Presence of antimicrobial activity in the urine reduces the bacterial load in these specimens. Hence, the chances of erroneously reporting insignificant bacteriuria can be reduced on analysis of the antimicrobial activity in urine. The aim of the study was to measure the antimicrobial activity of urine samples obtained from patients in a tertiary care hospital. A total of 100 urine specimens were collected from the study group. Tests like wet mount, Gram staining and culture were performed. Antimicrobial susceptibility testing was done on the bacteria isolated from each specimen. The urine specimens were reported as significant bacteriuria (>105 Colony Forming Unit (CFU)/ml) and insignificant bacteriuria (<105 CFU/ml - clean catch midstream urine; <102 CFU/ml - catheterized urine sample) according to the CFU/ml. Staphylococcus aureus ATCC(®) 25923(™) and Escherichia coli ATCC(®) 25922(™) were used to identify the presence of antimicrobial activity in the urine sample by Urine Anti-Bacterial substance Assay (UABA). McNemar test was used for statistical analysis using Statistical Package for the Social Sciences (SPSS) version 21.0. On analysis of the antimicrobial activity of urine sample with the prior antibiotic history of the patients, 17 were true positives and 43 were true negatives. Twenty six of samples with UABA positivity were culture negative and 28 samples with UABA positivity were culture positive. Sensitivity and specificity of the test was 85% and 53.8% respectively. Accuracy of the test was 60%. The p-value of UABA was <0.001. Enterobacteriaceae was the most common bacterial family isolated from the urine specimens. A total of 85% patients responded to treatment. Presence of antimicrobial activity in urine has a great impact on the interpretation of urine culture reports. Identification of urine antimicrobial activity

  4. NMR Chemical Shift Ranges of Urine Metabolites in Various Organic Solvents

    Directory of Open Access Journals (Sweden)

    Benjamin Görling

    2016-09-01

    Full Text Available Signal stability is essential for reliable multivariate data analysis. Urine samples show strong variance in signal positions due to inter patient differences. Here we study the exchange of the solvent of a defined urine matrix and how it affects signal and integral stability of the urinary metabolites by NMR spectroscopy. The exchange solvents were methanol, acetonitrile, dimethyl sulfoxide, chloroform, acetone, dichloromethane, and dimethyl formamide. Some of these solvents showed promising results with a single batch of urine. To evaluate further differences between urine samples, various acid, base, and salt solutions were added in a defined way mimicking to some extent inter human differences. Corresponding chemical shift changes were monitored.

  5. NMR Chemical Shift Ranges of Urine Metabolites in Various Organic Solvents

    Science.gov (United States)

    Görling, Benjamin; Bräse, Stefan; Luy, Burkhard

    2016-01-01

    Signal stability is essential for reliable multivariate data analysis. Urine samples show strong variance in signal positions due to inter patient differences. Here we study the exchange of the solvent of a defined urine matrix and how it affects signal and integral stability of the urinary metabolites by NMR spectroscopy. The exchange solvents were methanol, acetonitrile, dimethyl sulfoxide, chloroform, acetone, dichloromethane, and dimethyl formamide. Some of these solvents showed promising results with a single batch of urine. To evaluate further differences between urine samples, various acid, base, and salt solutions were added in a defined way mimicking to some extent inter human differences. Corresponding chemical shift changes were monitored. PMID:27598217

  6. Determination of flunixin in equine urine and serum by capillary electrophoresis.

    Science.gov (United States)

    Gu, X; Meleka-Boules, M; Chen, C L; Ceska, D M; Tiffany, D M

    1997-04-25

    A capillary electrophoresis (CE) and a solid-phase extraction method was developed for the determination of flunixin in equine urine and serum. The suitable CE run conditions were described. The factors affecting flunixin recovery rates were investigated and optimum solid-phase extraction conditions for flunixin in equine urine and serum were established. Limits of detection and quantitation were 3.4 and 5.6 ng/ml for serum and 16.9 and 33.1 ng/ml for urine, respectively. The recoveries exceeded 96% for urine and 79% for serum. Urine samples from race horses and urine and serum samples from a mare administrated with flunixin were analyzed with this procedure.

  7. Comparison of overnight, morning and 24-hour urine collections in the assessment of diabetic microalbuminuria

    DEFF Research Database (Denmark)

    Eshøj, O; Feldt-Rasmussen, B; Larsen, M L

    1987-01-01

    With the aim of comparing different urine collection periods in the assessment of micro-albuminuria, urinary albumin excretion rates (AERs) were measured in samples from 24 h, overnight, and morning urine collections in 54 patients aged 17 to 62 years with insulin-dependent diabetes mellitus...... with a mean duration of 15 years. The AER in overnight urine was found to be reduced by 25% compared to the rate in 24 h and morning urine. Assessing the ability to predict a 24 h AER within the microalbuminuric range (20-200 micrograms/min) we found a sensitivity of 90% and a specificity of 88% for both...... overnight and morning urine samples. These values were slightly improved by relating AE