WorldWideScience

Sample records for previously reported hplc

  1. [Electronic cigarettes - effects on health. Previous reports].

    Science.gov (United States)

    Napierała, Marta; Kulza, Maksymilian; Wachowiak, Anna; Jabłecka, Katarzyna; Florek, Ewa

    2014-01-01

    Currently very popular in the market of tobacco products have gained electronic cigarettes (ang. E-cigarettes). These products are considered to be potentially less harmful in compared to traditional tobacco products. However, current reports indicate that the statements of the producers regarding to the composition of the e- liquids not always are sufficient, and consumers often do not have reliable information on the quality of the product used by them. This paper contain a review of previous reports on the composition of e-cigarettes and their impact on health. Most of the observed health effects was related to symptoms of the respiratory tract, mouth, throat, neurological complications and sensory organs. Particularly hazardous effects of the e-cigarettes were: pneumonia, congestive heart failure, confusion, convulsions, hypotension, aspiration pneumonia, face second-degree burns, blindness, chest pain and rapid heartbeat. In the literature there is no information relating to passive exposure by the aerosols released during e-cigarette smoking. Furthermore, the information regarding to the use of these products in the long term are not also available.

  2. Transfusion Associated Peak in Hb HPLC Chromatogram – a Case Report

    Science.gov (United States)

    Jain, Sonal; Dass, Jasmita; Pati, Hara Prasad

    2012-01-01

    High performance liquid chromatography (HPLC) and electrophoresis are commonly used to diagnose various hemoglobinopathies. However, insufficient information about the transfusion history can lead to unexpected and confusing results. We are reporting a case of Juvenile myelomonocytic leukemia (JMML) in which HbHPLC was done to quantify fetal hemoglobin (HbF). The chromatogram showed elevated HbF along with a peak in the HbD window. A transfusion acquired peak was suspected based on the unexpectedly low percentage of HbD and was subsequently confirmed using parental HbHPLC. PMID:22348188

  3. Determination of Trace Elements in Uranium by HPLC-ID-ICP-MS: NTNFC Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Manard, Benjamin Thomas [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Wylie, Ernest Miller II [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Xu, Ning [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tandon, Lav [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-10-19

    This report covers the FY 16 effort for the HPLC-ID-ICP-MS methodology 1) sub-method validation for the group I&II elements, 2) sub-method stood-up and validation for REE, 3) sub-method development for the transition element, and 4) completion of a comprehensive SOP for three families of elements.

  4. Urethrotomy has a much lower success rate than previously reported.

    Science.gov (United States)

    Santucci, Richard; Eisenberg, Lauren

    2010-05-01

    We evaluated the success rate of direct vision internal urethrotomy as a treatment for simple male urethral strictures. A retrospective chart review was performed on 136 patients who underwent urethrotomy from January 1994 through March 2009. The Kaplan-Meier method was used to analyze stricture-free probability after the first, second, third, fourth and fifth urethrotomy. Patients with complex strictures (36) were excluded from the study for reasons including previous urethroplasty, neophallus or previous radiation, and 24 patients were lost to followup. Data were available for 76 patients. The stricture-free rate after the first urethrotomy was 8% with a median time to recurrence of 7 months. For the second urethrotomy stricture-free rate was 6% with a median time to recurrence of 9 months. For the third urethrotomy stricture-free rate was 9% with a median time to recurrence of 3 months. For procedures 4 and 5 stricture-free rate was 0% with a median time to recurrence of 20 and 8 months, respectively. Urethrotomy is a popular treatment for male urethral strictures. However, the performance characteristics are poor. Success rates were no higher than 9% in this series for first or subsequent urethrotomy during the observation period. Most of the patients in this series will be expected to experience failure with longer followup and the expected long-term success rate from any (1 through 5) urethrotomy approach is 0%. Urethrotomy should be considered a temporizing measure until definitive curative reconstruction can be planned. 2010 American Urological Association Education and Research, Inc. Published by Elsevier Inc. All rights reserved.

  5. Logic of Accounting: The Case of Reporting Previous Options in Norwegian Activation Encounters

    Science.gov (United States)

    Solberg, Janne

    2017-01-01

    The article deals with the enactment of client resistance in Norwegian vocational rehabilitation encounters. More specific, a practice here called "reporting previous options" is analyzed by using the resources of ethnomethodological conversation analysis (CA) in five instances as doing some sort of accounting. In response to the…

  6. Erysipelothrix endocarditis with previous cutaneous lesion: report of a case and review of the literature

    Directory of Open Access Journals (Sweden)

    Marion P. Rocha

    1989-08-01

    Full Text Available This report describes the first documented case of Erysipelothrix rhusiopathiae endocarditis in Latin America. The patient was a 51-years-old male, moderate alcoholic, with a previous history of aortic failure. He was used to fishing and cooking as a hobby and had his left hand wounded by a fish-bone. The disease began with erysipeloid form and developed to septicemia and endocarditis. He was treated with antibiotics and surgery for aortic valve replacement. There are only 46 cases of E. rhusiopathiae endocarditis reported to date. The authors wonder if several other cases might go unreported for lack of microbiological laboratorial diagnosis.

  7. Granulomatous lobular mastitis: report of a case with previously undescribed histopathological abnormalities.

    Science.gov (United States)

    Axelsen, R A; Reasbeck, P

    1988-10-01

    A 41-yr-old multiparous woman presented with a discrete breast lump which proved histologically to be an example of granulomatous lobular mastitis. The clinical and histological features were similar to those noted in previous reports. Additional histological features in the present case were an intense mononuclear cell infiltration of lobular and ductal epithelium, associated with nuclear fragments morphologically suggestive of apoptosis. These appearances, which have not previously been described, are illustrated, together with the more classical features of the condition well demonstrated by the present case. The novel histological features noted here suggest that the development of granulomatous lobular mastitis may be at least in part immunologically mediated, and that the cellular infiltrates seen may be a manifestation of cell-mediated destruction of mammary epithelium.

  8. Eikenella corrodens endocarditis and liver abscess in a previously healthy male, a case report

    DEFF Research Database (Denmark)

    Nordholm, Anne Christine; Vøgg, Ruth Ottilia Birgitta; Permin, Henrik

    2018-01-01

    BACKGROUND: Eikenella corrodens is one of the HACEK bacteria constituting part of the normal flora of the oropharynx, however, still an uncommon pathogen. We report a case of a large Eikenella corrodens liver abscess with simultaneously endocarditis in a previously healthy male. CASE PRESENTATION...... on pneumonia treatment, a PET-CT scan was performed, which showed a large multiloculated abscess in the liver. The abscess was drained using ultrasound guidance. Culture demonstrated Eikenella corrodens. Transesophageal echocardiography revealed aortic endocarditis. The patient was treated with antibiotics...... corrodens concurrent liver abscess and endocarditis. The case report highlights that Eikenella corrodens should be considered as a cause of liver abscess. Empirical treatment of pyogenic liver abscess will most often cover Eikenella corrodens, but the recommended treatment is a third generation...

  9. A previously unreported variant of the synostotic sagittal suture: Case report and review of salient literature

    Directory of Open Access Journals (Sweden)

    Madison Budinich

    2016-12-01

    Full Text Available Introduction: Sagittal synostosis is a rare congenital disease caused by the premature fusion of the sagittal suture. Craniosynostosis occurs for a variety of reasons, different for every case, and often the etiology is unclear but the anomaly can frequently be seen as part of Crouzon's or Apert's syndromes. Herein, we discuss a rare case of craniosynostosis where the patient presented with a, to our knowledge, a previously undescribed variant of sagittal synostosis. Case report: A 3-month-old female infant presented to a craniofacial clinic for a consultation regarding an abnormal head shape. Images of the skull were performed, demonstrating that the patient had craniosynostosis. The patient displayed no other significant symptoms besides abnormalities in head shape. The sagittal suture was found to extend into the occipital bone where it was synostotic. Conclusion: To our knowledge, a synostotic sagittal suture has not been reported that extended posteriorly it involve the occipital bone. Those who interpret imaging or operate on this part of the skull should consider such a variation. Keywords: Anatomy, Craniosynostosis, Skull, Malformation, Pediatrics

  10. Adenylosuccinate lyase (ADSL) and infantile autism: Absence of previously reported point mutation

    Energy Technology Data Exchange (ETDEWEB)

    Fon, E.A.; Sarrazin, J.; Rouleau, G.A. [Montreal General Hospital (Canada)] [and others

    1995-12-18

    Autism is a heterogeneous neuropsychiatric syndrome of unknown etiology. There is evidence that a deficiency in the enzyme adenylosuccinate lyase (ADSL), essential for de novo purine biosynthesis, could be involved in the pathogenesis of certain cases. A point mutation in the ADSL gene, resulting in a predicted serine-to-proline substitution and conferring structural instability to the mutant enzyme, has been reported previously in 3 affected siblings. In order to determine the prevalence of the mutation, we PCR-amplified the exon spanning the site of this mutation from the genomic DNA of patients fulfilling DSM-III-R criteria for autistic disorder. None of the 119 patients tested were found to have this mutation. Furthermore, on preliminary screening using single-strand conformation polymorphism (SSCP), no novel mutations were detected in the coding sequence of four ADSL exons, spanning approximately 50% of the cDNA. In light of these findings, it appears that mutations in the ADSL gene represent a distinctly uncommon cause of autism. 12 refs., 2 figs.

  11. Self-reported previous knee injury and low knee function increase knee injury risk in adolescent female football.

    Science.gov (United States)

    Clausen, M B; Tang, L; Zebis, M K; Krustrup, P; Hölmich, P; Wedderkopp, N; Andersen, L L; Christensen, K B; Møller, M; Thorborg, K

    2016-08-01

    Knee injuries are common in adolescent female football. Self-reported previous knee injury and low Knee injury and Osteoarthritis Outcome Score (KOOS) are proposed to predict future knee injuries, but evidence regarding this in adolescent female football is scarce. The aim of this study was to investigate self-reported previous knee injury and low KOOS subscale score as risk factors for future knee injuries in adolescent female football. A sample of 326 adolescent female football players, aged 15-18, without knee injury at baseline, were included. Data on self-reported previous knee injury and KOOS questionnaires were collected at baseline. Time-loss knee injuries and football exposures were reported weekly by answers to standardized text-message questions, followed by injury telephone interviews. A priori, self-reported previous knee injury and low KOOS subscale scores (female football. © 2015 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  12. A case report: mixed thrombus formation in a previously sutured right atrium.

    Science.gov (United States)

    Yunfei, Ling; Dongxu, Li; Shuhua, Luo; Yabo, Wang; San, Deep; Changping, Gan; Ke, Lin; Qi, An

    2014-08-01

    We describe the case of a 19-year-old Chinese woman who nine months prior underwent repair of an atrial septal defect and came to our hospital with a right atrial mass attached to the anterior wall of the right atrium on transthoracic echocardiography. Pathologic examination revealed the mass was a mixed-type thrombosis with some unusual organization, which previously was not described in literature.

  13. Health effects of low-level radiation in shipyard workers: report of previous work

    International Nuclear Information System (INIS)

    Matanoski, G.M.

    1984-01-01

    Progress over the course of the Nuclear Shipyard Workers Study is reported. The derivation of the study population, the gathering of health histories, the US Navy radiation protection program, and the determination of radiation exposures is described

  14. Absence of psilocybin in species of fungi previously reported to contain psilocybin and related tryptamine derivatives

    OpenAIRE

    Stijve, T.; Kuyper, Th.W.

    1988-01-01

    Seven taxa of agarics reported in literature to contain psilocybin (viz. Psathyrella candolleana, Gymnopilus spectabilis, G. fulgens, Hygrocybe psittacina var. psittacina and var. californica, Rickenella fibula, R. swartzii) have been analysed for psilocybin and related tryptamines with negative results.

  15. Absence of psilocybin in species of fungi previously reported to contain psilocybin and related tryptamine derivatives

    NARCIS (Netherlands)

    Stijve, T.; Kuyper, Th.W.

    1988-01-01

    Seven taxa of agarics reported in literature to contain psilocybin (viz. Psathyrella candolleana, Gymnopilus spectabilis, G. fulgens, Hygrocybe psittacina var. psittacina and var. californica, Rickenella fibula, R. swartzii) have been analysed for psilocybin and related tryptamines with negative

  16. Groin Problems in Male Soccer Players Are More Common Than Previously Reported

    DEFF Research Database (Denmark)

    Harøy, Joar; Clarsen, Ben; Thorborg, Kristian

    2017-01-01

    surveillance method developed to capture acute and overuse problems. STUDY DESIGN: Descriptive epidemiology study. METHODS: We registered groin problems during a 6-week period of match congestion using the Oslo Sports Trauma Research Center Overuse Injury Questionnaire. A total of 240 players from 15 teams......BACKGROUND: The majority of surveillance studies in soccer have used a time-loss injury definition, and many groin problems result from overuse, leading to gradually increasing pain and/or reduced performance without necessarily causing an absence from soccer training or match play. Thus......, the magnitude of groin problems in soccer has probably been underestimated in previous studies based on traditional injury surveillance methods. PURPOSE: To investigate the prevalence of groin problems among soccer players of both sexes and among male soccer players at different levels of play through a new...

  17. Alveolar nerve repositioning with rescue implants for management of previous treatment. A clinical report.

    Science.gov (United States)

    Amet, Edward M; Uehlein, Chris

    2013-12-01

    The goal of modern implant dentistry is to return patients to oral health in a rapid and predictable fashion, following a diagnostically driven treatment plan. If only a limited number of implants can be placed, or some fail and the prosthetic phase of implant dentistry is chosen to complete the patient's treatment, the final outcome may result in partial patient satisfaction and is commonly referred to as a "compromise." Previous All-on-4 implant treatment for the patient presented here resulted in a compromise, with an inadequate support system for the mandibular prosthesis and a maxillary complete denture with poor esthetics. The patient was unable to function adequately and also was disappointed with the resulting appearance. Correction of the compromised treatment consisted of bilateral inferior alveolar nerve elevation and repositioning without bone removal for lateral transposition, to gain room for rescue implants for a totally implant-supported and stabilized prosthesis. Treatment time to return the patient to satisfactory comfort, function, facial esthetics, and speech was approximately 2 weeks. The definitive mandibular prosthesis was designed for total implant support and stability with patient retrievability. Adequate space between the mandibular bar system and the soft tissue created a high water bridge effect for self-cleansing. Following a short interim mandibular healing period, the maxillary sinuses were bilaterally grafted to compensate for bone inadequacies and deficiencies for future maxillary implant reconstruction. © 2013 by the American College of Prosthodontists.

  18. [Lessons from abroad. Current and previous crisis in other countries. SESPAS report 2014].

    Science.gov (United States)

    Rivadeneyra-Sicilia, Ana; Minué Lorenzo, Sergio; Artundo Purroy, Carlos; Márquez Calderón, Soledad

    2014-06-01

    The evidence available on the impact of previous crises on health reveals different patterns attributable to study designs, the characteristics of each crisis, and other factors related to the socioeconomic and political context. There is greater consensus on the mediating role of government policy responses to financial crises. These responses may magnify or mitigate the adverse effects of crises on population health. Some studies have shown a significant deterioration in some health indicators in the context of the current crisis, mainly in relation to mental health and communicable diseases. Alcohol and tobacco use have also declined in some European countries. In addition, this crisis is being used by some governments to push reforms aimed at privatizing health services, thereby restricting the right to health and healthcare. Specifically, action is being taken on the three axes that determine health system financing: the population covered, the scope of services, and the share of the costs covered. These measures are often arbitrarily implemented based on ideological decisions rather than on the available evidence and therefore adverse consequences are to be expected in terms of financial protection, efficiency, and equity. Copyright © 2013 SESPAS. Published by Elsevier Espana. All rights reserved.

  19. Increased Symptom Reporting in Young Athletes Based on History of Previous Concussions.

    Science.gov (United States)

    Moser, Rosemarie Scolaro; Schatz, Philip

    2017-01-01

    Research documents increased symptoms in adolescents with a history of two or more concussions. This study examined baseline evaluations of 2,526 younger athletes, ages 10 to 14. Between-groups analyses examined Post Concussion Symptom Scale symptoms by concussion history group (None, One, Two+) and clusters of Physical, Cognitive, Emotional, and Sleep symptoms. Healthy younger athletes with a concussion history reported greater physical, emotional, and sleep-related symptoms than those with no history of concussion, with a greater endorsement in physical/sleep symptom clusters. Findings suggest younger athletes with a history of multiple concussions may experience residual symptoms.

  20. Leiomyosarcoma of the Prostate: Case Report and Review of 54 Previously Published Cases

    Directory of Open Access Journals (Sweden)

    Gerasimos P. Vandoros

    2008-01-01

    Full Text Available Prostate leiomyosarcoma is an extremely rare and highly aggressive neoplasm that accounts for less than 0.1% of primary prostate malignancies. We present a patient with primary leiomyosarcoma of the prostate and review 54 cases reported in the literature to discuss the clinical, diagnostic and therapeutic aspects of this uncommon tumor. Median survival was estimated at 17 months (95% C.I. 20.7–43.7 months and the 1-, 3-, and 5-year actuarial survival rates were 68%, 34%, and 26%, respectively. The only factors predictive of long-term survival were negative surgical margins and absence of metastatic disease at presentation. A multidisciplinary approach is necessary for appropriate management of this dire entity.

  1. Acquisition of HPLC-Mass Spectrometer

    Science.gov (United States)

    2015-08-18

    31-Jan-2015 Approved for Public Release; Distribution Unlimited Final Report: Acquisition of HPLC -Mass Spectrometer The views, opinions and/or findings...published in peer-reviewed journals: Final Report: Acquisition of HPLC -Mass Spectrometer Report Title The acquisition of the mass spectrometer has been a

  2. Ruptured Rudimentary Horn Pregnancy at 25 Weeks with Previous Vaginal Delivery: A Case Report

    Directory of Open Access Journals (Sweden)

    Deepa V. Kanagal

    2012-01-01

    Full Text Available Unicornuate uterus with rudimentary horn occurs due to failure of complete development of one of the Mullerian ducts and incomplete fusion with the contralateral side. Pregnancy in a noncommunicating rudimentary horn is extremely rare and usually terminates in rupture during first or second trimester of pregnancy. Diagnosis of rudimentary horn pregnancy and its rupture in a woman with prior vaginal delivery is difficult. It can be missed in routine ultrasound scan and in majority of cases it is detected after rupture. It requires a high index of suspicion. We report a case of G2PlL1 with rupture rudimentary horn pregnancy at 25 weeks of gestation which was misdiagnosed as intrauterine pregnancy with fetal demise by ultrasound, and termination was attempted and the case was later referred to our hospital after the patient developed hemoperitoneum and shock with a diagnosis of rupture uterus. Laparotomy revealed rupture of right rudimentary horn pregnancy with massive hemoperitoneum. Timely laparotomy, excision of the horn, and blood transfusion saved the patient.

  3. Stevens-Johnson Syndrome Induced by Carbamazepine Treatment in a Patient Who Previously Had Carbamazepine Induced Pruritus - A Case Report -

    OpenAIRE

    Bae, Hyun Min; Park, Yoo Jung; Kim, Young Hoon; Moon, Dong Eon

    2013-01-01

    Stevens-Johnson syndrome (SJS) is a rare but life-threatening skin reaction disease and carbamazepine is one of its most common causes. We report a case of SJS secondary to carbamazepine in a patient with previous pruritus due to carbamazepine which was given for treatment of trigeminal neuralgia. We would like to caution all providers that carbamazepine readministration should be avoided in the patient with a previous history of SJS or adverse skin reaction. In addition, we strongly recommen...

  4. Self-reported previous knee injury and low knee function increase knee injury risk in adolescent female football

    DEFF Research Database (Denmark)

    Clausen, Mikkel Bek; Tang, L; Zebis, M K

    2016-01-01

    with low KOOS subscale scores (Sport/Recreational (RR: 2.2) and Quality of Life (RR: 3.0) (P time-loss knee...... questionnaires were collected at baseline. Time-loss knee injuries and football exposures were reported weekly by answers to standardized text-message questions, followed by injury telephone interviews. A priori, self-reported previous knee injury and low KOOS subscale scores (... as independent variables in the risk factor analyses. The study showed that self-reported previous knee injury significantly increased the risk of time-loss knee injury [relative risk (RR): 3.65, 95% confidence (CI) 1.73-7.68; P time-loss knee injury was also significantly increased in players...

  5. Lack of Cetuximab induced skin toxicity in a previously irradiated field: case report and review of the literature

    Science.gov (United States)

    2010-01-01

    Introduction Mutation, amplification or dysregulation of the EGFR family leads to uncontrolled division and predisposes to cancer. Inhibiting the EGFR represents a form of targeted cancer therapy. Case report We report the case of 79 year old gentlemen with a history of skin cancer involving the left ear who had radiation and surgical excision. He had presented with recurrent lymph node in the left upper neck. We treated him with radiation therapy concurrently with Cetuximab. He developed a skin rash over the face and neck area two weeks after starting Cetuximab, which however spared the previously irradiated area. Conclusion The etiology underlying the sparing of the previously irradiated skin maybe due to either decrease in the population of EGFR expressing cells or decrease in the EGFR expression. We raised the question that "Is it justifiable to use EGFR inhibitors for patients having recurrence in the previously irradiated field?" We may need further research to answer this question which may guide the physicians in choosing appropriate drug in this scenario. PMID:20478052

  6. Shunt malfunction causing acute neurological deterioration in 2 patients with previously asymptomatic Chiari malformation Type I. Report of two cases.

    Science.gov (United States)

    Elliott, Robert; Kalhorn, Stephen; Pacione, Donato; Weiner, Howard; Wisoff, Jeffrey; Harter, David

    2009-08-01

    Patients with symptomatic Chiari malformation Type I (CM-I) typically exhibit a chronic, slowly progressive disease course with evolution of symptoms. However, some authors have reported acute neurological deterioration in the setting of CM-I and acquired Chiari malformations. Although brainstem dysfunction has been documented in patients with CM-II and hydrocephalus or shunt malfunction, to the authors' knowledge only 1 report describing ventriculoperitoneal (VP) shunt malfunction causing neurological deterioration in a patient with CM-I exists. The authors report on their experience with the treatment of previously asymptomatic CM-I in 2 children who experienced quite different manifestations of acute neurological deterioration secondary to VP shunt malfunction. Presumably, VP shunt malfunction created a positive rostral pressure gradient across a stenotic foramen magnum, resulting in tetraparesis from foramen magnum syndrome in 1 patient and acute ataxia and cranial nerve deficits from syringobulbia in the other. Although urgent shunt revisions yielded partial recovery of neurological function in both patients, marked improvement occurred only after posterior fossa decompression.

  7. Placenta Percreta Invading Broad Ligament and Parametrium in a Woman with Two Previous Cesarean Sections: A Case Report

    Directory of Open Access Journals (Sweden)

    Mansoureh Vahdat

    2012-01-01

    Full Text Available Introduction. The incidence of placenta accreta has dramatically increased due to increasing caesarean section rate all over the world. Placenta percreta is the most severe form of placenta accretes. It frequently results in maternal morbidity and mortality mainly caused by massive obstetric hemorrhage or emergency hysterectomy. Percreta invading into the broad ligament has rarely been previously reported. Case presenting. We presented a case of placenta percreta invading left broad ligament and parametrium in a woman with two previous cesarean sections, which led to massive intraoperative hemorrhage during hysterectomy and transient ischemic encephalopathy. Conclusion. In cases of parametrial involvement, it would be more difficult to decide whether to remove placenta or leave it in site. In surgical removal neither local excision of placental bed and uterine repair nor traditional hysterectomy is adequate if parametrium invaded by placenta. We suggest delayed elective hysterectomy in such cases. So, pregnancy-induced pelvic congestion would be decreased, we can gather an expert team of gynecologists, urologists, and vascular surgeons, we could get plenty of blood products, and we may have the chance to administer methotrexate.

  8. [Double mutant alleles in the EXT1 gene not previously reported in a teenager with hereditary multiple exostoses].

    Science.gov (United States)

    Cammarata-Scalisi, Francisco; Cozar, Mónica; Grinberg, Daniel; Balcells, Susana; Asteggiano, Carla G; Martínez-Domenech, Gustavo; Bracho, Ana; Sánchez, Yanira; Stock, Frances; Delgado-Luengo, Wilmer; Zara-Chirinos, Carmen; Chacín, José Antonio

    2015-04-01

    Hereditary forms of multiple exostoses, now called EXT1/EXT2-CDG within Congenital Disorders of Glycosylation, are the most common benign bone tumors in humans and clinical description consists of the formation of several cartilage-capped bone tumors, usually benign and localized in the juxta-epiphyseal region of long bones, although wide body dissemination in severe cases is not uncommon. Onset of the disease is variable ranging from 2-3 years up to 13-15 years with an estimated incidence ranging from 1/18,000 to 1/50,000 cases in European countries. We present a double mutant alleles in the EXT1 gene not previously reported in a teenager and her family with hereditary multiple exostoses.

  9. Pushing the boundaries in liver graft utilisation in transplantation: Case report of a donor with previous bile duct injury repair.

    Science.gov (United States)

    Sultana, Asma; Powell, James J; Oniscu, Gabriel C

    2017-01-01

    Liver transplantation is a recognised treatment for extensive bile duct injuries with secondary biliary cirrhosis or recurring sepsis. However, there have been no reports of successful liver transplantation from a donor who sustained a previous bile duct injury. Here we discuss the case of a liver transplant from a 51-year-old brain dead donor who had suffered a Strasberg E1 bile duct injury and had undergone a Roux-en-Y hepaticojejunostomy 24 years prior to donation. The liver was successfully recovered and transplanted into a 56-year-old male recipient with end stage liver disease consequent to alpha 1 antitrypsin deficiency. The graft continues to function well 36 months post-transplant, with normal liver function tests and imaging revealing a patent hepaticojejunostomy. The potential associated vascular injuries should be identified during bench preparation whilst the management of biliary reconstruction at the time of transplant should follow the principles of biliary reconstruction in cases with biliary injuries, extending the hilar opening into the left duct. This case highlights the successful utilisation of a post bile duct injury repair liver, employing an experienced procurement team and careful bench assessment and reconstruction. Copyright © 2017. Published by Elsevier Ltd.

  10. External cephalic version among women with a previous cesarean delivery: report on 36 cases and review of the literature.

    Science.gov (United States)

    Abenhaim, Haim A; Varin, Jocelyne; Boucher, Marc

    2009-01-01

    Whether or not women with a previous cesarean section should be considered for an external cephalic version remains unclear. In our study, we sought to examine the relationship between a history of previous cesarean section and outcomes of external cephalic version for pregnancies at 36 completed weeks of gestation or more. Data on obstetrical history and on external cephalic version outcomes was obtained from the C.H.U. Sainte-Justine External Cephalic Version Database. Baseline clinical characteristics were compared among women with and without a history of previous cesarean section. We used logistic regression analysis to evaluate the effect of previous cesarean section on success of external cephalic version while adjusting for parity, maternal body mass index, gestational age, estimated fetal weight, and amniotic fluid index. Over a 15-year period, 1425 external cephalic versions were attempted of which 36 (2.5%) were performed on women with a previous cesarean section. Although women with a history of previous cesarean section were more likely to be older and para >2 (38.93% vs. 15.0%), there were no difference in gestational age, estimated fetal weight, and amniotic fluid index. Women with a prior cesarean section had a success rate similar to women without [50.0% vs. 51.6%, adjusted OR: 1.31 (0.48-3.59)]. Women with a previous cesarean section who undergo an external cephalic version have similar success rates than do women without. Concern about procedural success in women with a previous cesarean section is unwarranted and should not deter attempting an external cephalic version.

  11. Sensitive detectors in HPLC

    International Nuclear Information System (INIS)

    Anon.

    1992-01-01

    Detection of sample components in HPLC is difficult for many reasons; the key difficulty is the mobile phase which usually has properties similar to the solute. A variety of detectors have been developed for use in HPLC based on one of the above approaches; however, the search is still continuing for an ideal or universal detector. A universal detector should have the following characteristics: (1) responds to all solutes or has predictable specificity; (2) high detectability and the same predictable response; (3) fast response; (4) wide range of linearity; (5) unaffected by changes in temperature and mobile-phase flow; (6) responds independently of the mobile phase; (7) makes no contribution to extracolumn band broadening; (8) reliable and convenient to use; (9) nondestructive to the solute; (10) provides qualitative information on the detected peak. Unfortunately, no available HPLC detector possesses all these properties. 145 refs

  12. The Natural History of Juvenile or Subacute GM2 Gangliosidosis: 21 New Cases and Literature Review of 134 Previously Reported

    Science.gov (United States)

    Maegawa, Gustavo H. B.; Stockley, Tracy; Tropak, Michael; Banwell, Brenda; Blaser, Susan; Kok, Fernando; Giugliani, Roberto; Mahuran, Don; Clarke, Joe T. R.

    2010-01-01

    OBJECTIVE Juvenile GM2 gangliosidosis is a group of inherited neurodegenerative diseases caused by deficiency of lysosomal β-hexosaminidase resulting in GM2 ganglioside accumulation in brain. The purpose of this study was to delineate the natural history of the condition and identify genotype-phenotype correlations that might be helpful in predicting the course of the disease in individual patients. METHODS A cohort of 21 patients with juvenile GM2 gangliosidosis, 15 with the Tay-Sachs variant and 6 with the Sandhoff variant, was studied prospectively in 2 centers. Our experience was compared with previously published reports on 134 patients. Information about clinical features, β-hexosaminidase enzyme activity, and mutation analysis was collected. RESULTS In our cohort of patients, the mean (±SD) age of onset of symptoms was 5.3 ± 4.1 years, with a mean follow-up time of 8.4 years. The most common symptoms at onset were gait disturbances (66.7%), incoordination (52.4%), speech problems (28.6%), and developmental delay (28.6%). The age of onset of gait disturbances was 7.1 ± 5.6 years. The mean time for progression to becoming wheelchair-bound was 6.2 ± 5.5 years. The mean age of onset of speech problems was 7.0 ± 5.6 years, with a mean time of progression to anarthria of 5.6 ± 5.3 years. Muscle wasting (10.6 ± 7.4 years), proximal weakness (11.1 ± 7.7 years), and incontinence of sphincters (14.6 ± 9.7 years) appeared later in the course of the disease. Psychiatric disturbances and neuropathy were more prevalent in patients with the Sandhoff variant than in those with the Tay-Sachs variant. However, dysphagia, sphincter incontinence, and sleep problems occurred earlier in those with the Tay-Sachs variant. Cerebellar atrophy was the most common finding on brain MRI (52.9%). The median survival time among the studied and reviewed patients was 14.5 years. The genotype-phenotype correlation revealed that in patients with the Tay-Sachs variant, the presence

  13. Analysis of over 10,000 Cases finds no association between previously reported candidate polymorphisms and ovarian cancer outcome

    DEFF Research Database (Denmark)

    White, Kristin L; Vierkant, Robert A; Fogarty, Zachary C

    2013-01-01

    Ovarian cancer is a leading cause of cancer-related death among women. In an effort to understand contributors to disease outcome, we evaluated single-nucleotide polymorphisms (SNP) previously associated with ovarian cancer recurrence or survival, specifically in angiogenesis, inflammation, mitosis...

  14. Rib cage deformity during two-stage tissue expander breast reconstruction in patient with previous radiotherapy: a case report

    Directory of Open Access Journals (Sweden)

    Aleš Porčnik

    2016-02-01

    Full Text Available Patients undergoing two-stage breast reconstruction with tissue expander and a history of previous irradiation are predisposed to a various chest-wall deformations more than non-irradiated patients. If chest-wall depression with/without rib fracture is found intra-operatively, bigger implant should be used, with a subsequent radiologic evaluation. In the future, the development of a new, modified expander with a harder base could minimise such complications.

  15. A Case Report of Salmonella muenchen Enteritis Causing Rhabdomyolysis and Myocarditis in a Previously Healthy 26-Year-Old Man.

    Science.gov (United States)

    Chapple, Will; Martell, Jon; Wilson, Joy S; Matsuura, Don T

    2017-04-01

    This case report examines an unusual presentation of a non-typhoidal Salmonella serovar with limited prevalence in the literature. This is the first case report to associate specifically the Salmonella muenchen serovar with rhabdomyolysis and myocarditis. This case report reviews the diagnostic criteria for myocarditis and explores the diagnostic dilemma of troponin elevation in the setting of rhabdomyolysis. It demonstrates that Salmonella muenchen has the ability to present in a broad range of individuals with complications extending beyond classical gastrointestinal symptoms. This report also concludes that diagnosis of the many possible complications from non-typhoidal Salmonella infections can be difficult due to patient comorbidities, variability in the severity of the illnesses, laboratory test limitations, and imaging limitations. When a patient presents with elevated troponins in the setting of rhabdomyolysis a careful workup should be done to evaluate for ischemic causes, myocarditis, or false elevation secondary to rhabdomyolysis.

  16. Continuation of the summarizing interim report on previous results of the Gorleben site survey as of May 1983

    International Nuclear Information System (INIS)

    1990-04-01

    In addition to results from the 1983 interim report, this report contains, in order to supplement the surface explorations, seismic reflection measurements, hydrogeologic and seismologic investigations, sorption experiments, and studies of glacial development in the site region and of long-term safety of final waste repositories in salt domes. The site's high grade of suitability for becoming a final radioactive waste repository, the legal basis as well as quality assurance are evaluated. (orig.) [de

  17. 24 CFR 1710.558 - Previously accepted state filings-notice of revocation rights on property report cover page.

    Science.gov (United States)

    2010-04-01

    ... will give the purchaser written notification of purchaser's default or breach of contract and the... purchaser loses rights and interest in the lot because of the purchaser's default or breach of contract... Report prior to signing a contract or agreement, you may cancel your contract or agreement by giving...

  18. Leptotrichia endocarditis: report of two cases from the International Collaboration on Endocarditis (ICE) database and review of previous cases

    NARCIS (Netherlands)

    Caram, L. B.; Linefsky, J. P.; Read, K. M.; Murdoch, D. R.; Lalani, T.; Woods, C. W.; Reller, L. B.; Kanj, S. S.; Premru, M. M.; Ryan, S.; Al-Hegelan, M.; Donnio, P. Y.; Orezzi, C.; Paiva, M. G.; Tribouilloy, C.; Watkin, R.; Harris, O.; Eisen, D. P.; Corey, G. R.; Cabell, C. H.; Petti, C. A.; Gordon, David; Devi, Uma; Spelman, Denis; van der Meer, Jan T. M.; Kauffman, Carol; Bradley, Suzanne; Armstrong, William; Giannitsioti, Efthymia; Giamarellou, Helen; Lerakis, Stamatios; del Rio, Ana; Moreno, Asuncion; Mestres, Carlos A.; Paré, Carlos; de la Maria, Cristina Garcia; de Lazzario, Elisa; Marco, Francesc; Gatell, Jose M.; Miró, José M.; Almela, Manel; Azqueta, Manuel; Jiménez-Expósito, Maria Jesús; de Benito, Natividad; Perez, Noel; Almirante, Benito; Fernandez-Hidalgo, Nuria; de Vera, Pablo Rodriguez; Tornos, Pilar; Falcó, Vicente

    2008-01-01

    Leptotrichia species typically colonize the oral cavity and genitourinary tract. We report the first two cases of endocarditis secondary to L. goodfellowii sp. nov. Both cases were identified using 16S rRNA gene sequencing. Review of the English literature revealed only two other cases of

  19. Case report of electronic cigarettes possibly associated with eosinophilic pneumonitis in a previously healthy active-duty sailor.

    Science.gov (United States)

    Thota, Darshan; Latham, Emi

    2014-07-01

    Electronic cigarettes (e-cigarettes) are a technology that has been touted as a safe and effective alternative to traditional cigarettes. There is, however, a paucity of literature showing the adverse outcomes of e-cigarettes and a correlation with acute eosinophilic pneumonia (AEP). To present a possible association between e-cigarettes and AEP. A 20-year-old previously healthy man was found to develop AEP after smoking an e-cigarette. He was treated with antibiotics and steroids and his symptoms improved. Though an alternative to traditional cigarettes, e-cigarettes can have unpredictable and potentially serious adverse effects. More research needs to be conducted to determine their safety. If seeing a patient in the ED with pulmonary symptoms after use of e-cigarettes, AEP should be considered in the differential. Published by Elsevier Inc.

  20. Central posterior capsule pigmentation in a patient with pigment dispersion and previous ocular trauma: a case report.

    Science.gov (United States)

    Al-Mezaine, Hani S

    2010-01-01

    We report a 55-year-old man with unusually dense, unilateral central posterior capsule pigmentation associated with the characteristic clinical features of pigment dispersion syndrome, including a Krukenberg's spindle and dense trabecular pigmentation in both eyes. A history of an old blunt ocular trauma probably caused separation of the anterior hyaloid from the back of the lens, thereby creating an avenue by which pigment could reach the potential space of Berger's from the posterior chamber.

  1. Central posterior capsule pigmentation in a patient with pigment dispersion and previous ocular trauma: A case report

    Directory of Open Access Journals (Sweden)

    Al-Mezaine Hani

    2010-01-01

    Full Text Available We report a 55-year-old man with unusually dense, unilateral central posterior capsule pigmentation associated with the characteristic clinical features of pigment dispersion syndrome, including a Krukenberg′s spindle and dense trabecular pigmentation in both eyes. A history of an old blunt ocular trauma probably caused separation of the anterior hyaloid from the back of the lens, thereby creating an avenue by which pigment could reach the potential space of Berger′s from the posterior chamber.

  2. Unexpected finding of T-cell lymphoma in a previously healthy 16-year-old patient after a thorax trauma: a case report

    DEFF Research Database (Denmark)

    Bach Okholm-Hansen, Anna; Brorson, Stig

    2014-01-01

    INTRODUCTION: We describe the clinical course and emphasize the difficulties in diagnosing T-cell lymphoblastic lymphoma. The differential diagnostic difficulties have previously been described in regard to pneumonia, but to the best of the authors' knowledge this is the first case report to desc...... relevant to pediatricians, surgeons, anesthesiologists, and general practitioners....

  3. On-line radioactivity detector for HPLC

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1986-01-01

    Over the last ten years the technique of high performance liquid chromotography (HPLC) has become extensively employed for the separation and quantitation of various biological, organic, and inorganic substances. The use of HPLC for the separation of various metabolic compounds has become routine. The major problem of analyzing the metabolism process is that the quantitation is accomplished by the use of radioactive substrates. Until recently the only method to quantitate these radioactive compounds eluting from the HPLC was by collecting fractions at preset times, removing aliquots and quantitating in a liquid scintillation counter. Once the radioactivity present in each fraction was determined, the results were plotted on a graph and the area of each of the radioactive peaks was determined. This entire process required from 3-20 hours. The introduction of the flow through radioactivity detector enable the investigator to directly quantitate the radioactive peaks as they elute from the HPLC in real time and at about one-tenth the original cost of the previous methods. The detection limits of this technique are dependent on the residence time of the sample in the flow cell and the type of flow cell used for the analysis. Using a 2.5 ml liquid flow cell, (mixing with liquid scintillation solution), base line resolution can be obtained for peaks 1.5 minutes apart, and a sensitivity of 70 dpm for tritium and 30 dpm for carbon-14 can be achieved

  4. Determination of blood cyanide by HPLC-MS.

    Science.gov (United States)

    Tracqui, A; Raul, J S; Géraut, A; Berthelon, L; Ludes, B

    2002-04-01

    An original high-performance liquid chromatographic-mass spectrometric (HPLC-MS) procedure was developed for the determination of cyanide (CN) in whole blood. After the addition of K13C15N as internal standard, blood was placed in a microdiffusion device, the inner well of which was filled with a mixture of taurine (50mM in water)/naphthalene-2,3-dicarboxaldehyde (NDA, 10mM in methanol)/methanol/ concentrated (approximately 20%) ammonia solution (25:25:45:5, v/v). Concentrated H2SO4 was added to the blood sample, and the microdiffusion chamber was sealed. After 30 min of gentle agitation, 2 microL of the contents of the inner vial were pipetted and directly injected onto a NovaPak C18 HPLC column. Separation was performed by a gradient of acetonitrile in 2mM NH4COOH, pH 3.0 buffer (35-80% in 10 min). Detection was done with a Perkin-Elmer Sciex API-100 mass analyzer with an ionspray interface, operated in the negative ionization mode. MS data were collected as either TIC or SIM at m/z (299 + 191) and (301 + 193) for the derivatives formed with CN and 13C15N, respectively. Inspired by previous works dealing with the complexation of CN by NDA + taurine to form a 1-cyano [f] benzoisoindole derivative analyzed by HPLC-fluorimetry, this method appears simple, rapid, and extremely specific. Limits of detection and quantitation for blood CN are 5 and 15 ng/mL, respectively. The use of 13C15N as internal standard allows the quantitation of CN with elegance and accuracy in comparison with previously reported methods.

  5. HPLC: Early and Recent Perspectives.

    Science.gov (United States)

    Karger, Barry L.

    1997-01-01

    Provides a perspective on what it was like in the early days of high-performance liquid chromatography (HPLC) and several of the key developments. Focuses on the advances in HPLC generally, and more specifically for the biological sciences, that were necessary for the method to reach the preeminent stage of today. Contains 20 references. (JRH)

  6. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasawa, Koji, E-mail: koji180@pharm.showa-u.ac.jp; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-02-15

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H{sub 2}O{sub 2} and O{sub 2}{sup −} generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  7. Novel assay of antibacterial components in manuka honey using lucigenin-chemiluminescence-HPLC

    International Nuclear Information System (INIS)

    Karasawa, Koji; Haraya, Shiomi; Okubo, Sachie; Arakawa, Hidetoshi

    2017-01-01

    Five components (hydrogen peroxide, methylglyoxal, dihydroxyacetone, fructose and glucose) of New Zealand manuka honey (Leptospermum scoparium) were analyzed using lucigenin chemiluminescence high-performance liquid chromatography (lucigenin-CL-HPLC). We focused on active oxygen species produced from the components in order to easily detect these five components contained in manuka honey. H_2O_2 and O_2"− generated from these components were identified by lucigenin-CL and electron spin resonance (ESR), and the bactericidal effect of ROS was confirmed using E. coli. The previously reported assays for Manuka honey components have low specificities and require complicated preprocessing methods. As our results, the detection and identification of these components were possible within 30 min in lucigenin-CL-HPLC system, without any special treatment. It is considered that lucigenin-CL-HPLC is useful for the quality control and the analysis of various honey. - Highlights: • Antibacterial components in manuka honey by HPLC with lucigenin-CL. • Five antibacterial compounds measured via generation of reactive oxygen species. • Simple, sensitive and useful for quality control and analysis of antibacterial honey.

  8. [Metatropic dysplasia in a girl with c.1811_1812delinsAT mutation in exon 11 of the TRPV4 gene not previously reported].

    Science.gov (United States)

    Cammarata-Scalisi, Francisco; Matysiak-Scholze, Uta; Heinze, Jessica; Barrera, Albaro; Lacruz-Rengel, María Angelina; Bracho, Ana; Guerrero, Yudith

    2015-01-01

    Metatropic dysplasia is a skeletal disorder with clinical heterogeneity, characterized by craniofacial dysmorphy including frontal bossing and midface hypoplasia, short trunk,progressive kyphoscoliosis and shortened limbs. The TRPV4 gene is located on 12q24.11, coding a cation channel with nonselective permeability to calcium; it is expressed and involved in many physiological processes through responses to different stimuli. Over 50 mutations in TRPV4 have been described. We present a seven months old girl with heterozygous mutation c.1811_1812delinsAT; p.I604N in intron 11 not previously reported in the TRPV4 gene and with clinical findings compatible with metatropic dysplasia.

  9. New Record of Sillago sinica (Pisces: Sillaginidae in Korean Waters, and Re-identification of Sillago parvisquamis Previously Reported from Korea as S. sinica

    Directory of Open Access Journals (Sweden)

    Seung Eun Bae

    2013-10-01

    Full Text Available A single specimen of the genus Sillago, collected from Gwangyang, Korea, in May 2009, is characterized by XI first dorsal fin spines, 3 or 4 rows of melanophore pattern along the second dorsal fin membrane, and a darkish posterior margin of the caudal fin. Our specimen was identified as Sillago sinica reported as a new species; this identification is confirmed by mitochondrial DNA cytochrome oxidase subunit I sequences, which show that our specimen corresponds to S. sinica (d=0.000 and differs from the congeneric species Sillago parvisquamis (d=0.170. Comparisons of Korean specimens previously reported as S. parvisquamis with specimens of S. sinica show that the S. parvisquamis specimens are actually S. sinica. We propose the new Korean name “buk-bang-jeom-bo-ri-myeol” for S. sinica.

  10. Prospective evaluation of patient-reported quality-of-life outcomes following SBRT ± cetuximab for locally-recurrent, previously-irradiated head and neck cancer

    International Nuclear Information System (INIS)

    Vargo, John A.; Heron, Dwight E.; Ferris, Robert L.; Rwigema, Jean-Claude M.; Wegner, Rodney E.; Kalash, Ronny; Ohr, James; Kubicek, Greg J.; Burton, Steven

    2012-01-01

    Purpose: Stereotactic body radiotherapy (SBRT) has emerged as a promising salvage strategy for unresectable, previously-irradiated recurrent squamous cell carcinomas of the head and neck (rSCCHN). Here-in, we report the first prospective evaluation of patient-reported quality-of-life (PR-QoL) following re-irradiation with SBRT ± cetuximab for rSCCHN. Materials and methods: From November 2004 to May 2011, 150 patients with unresectable, rSCCHN in a previously-irradiated field receiving >40 Gy were treated with SBRT to 40–50 Gy in 5 fractions ± concurrent cetuximab. PR-QoL was prospectively acquired using University of Washington Quality-of-Life Revised (UW-QoL-R). Results: Overall PR-QoL, health-related PR-QoL, and select domains commonly affected by re-irradiation progressively increase following an initial 1-month decline with statistically significant improvements noted in swallowing (p = 0.025), speech (p = 0.017), saliva (p = 0.041), activity (p = 0.032) and recreation (p = 0.039). Conclusions: Especially for patients surviving >1-year, improved tumor control associated with SBRT re-irradiation may ameliorate decreased PR-QoL resulting from rSCCHN. These improvements in PR-QoL transcend all measured domains in a validated PR-QoL assessment tool independent of age, use of cetuximab, tumor volume, and interval since prior irradiation.

  11. Prospective monitoring and self-report of previous falls among older women at high risk of falls and fractures: a study of comparison and agreement.

    Science.gov (United States)

    Garcia, Patrícia A; Dias, João M D; Silva, Silvia L A; Dias, Rosângela C

    2015-01-01

    The identification of the occurrence of falls is an important step for screening and for rehabilitation processes for the elderly. The methods of monitoring these events are susceptible to recording biases, and the choice of the most accurate method remains challenging. (i) To investigate the agreement between retrospective self-reporting and prospective monitoring of methods of recording falls, and (ii) to compare the retrospective self-reporting of falls and the prospective monitoring of falls and recurrent falls over a 12-month period among older women at high risk of falls and fractures. A total of 118 community-dwelling older women with low bone density were recruited. The incidence of falls was monitored prospectively in 116 older women (2 losses) via monthly phone calls over the course of a year. At the end of this monitoring period, the older women were asked about their recall of falls in the same 12-month period. The agreement between the two methods was analyzed, and the sensitivity and specificity of self-reported previous falls in relation to the prospective monitoring were calculated. There was moderate agreement between the prospective monitoring and the retrospective self-reporting of falls in classifying fallers (Kappa = 0.595) and recurrent fallers (Kappa = 0.589). The limits of agreement were 0.35 ± 1.66 falls. The self-reporting of prior falls had a 67.2% sensitivity and a 94.2% specificity in classifying fallers among older women and a 50% sensitivity and a 98.9% specificity in classifying recurrent fallers. Self-reporting of falls over a 12-month period underestimated 32.8% of falls and 50% of recurrent falls. The findings recommend caution if one is considering replacing monthly monitoring with annual retrospective questioning.

  12. An Investigation Into HPLC Data Quality Problems

    Science.gov (United States)

    Hooker, Stanford B.; VanHeukelem, Laurie

    2011-01-01

    This report summarizes the analyses and results produced by a five-member investigative team of Government, university, and industry experts, established by NASA HQ. The team examined data quality problems associated with high performance liquid chromatography (HPLC) analyses of pigment concentrations in seawater samples produced by the San Diego State University (SDSU) Center for Hydro-Optics and Remote Sensing (CHORS). This report shows CHORS did not validate the methods used before placing them into service to analyze field samples for NASA principal investigators (PIs), even though the HPLC literature contained easily accessible method validation procedures, and the importance of implementing them, more than a decade ago. In addition, there were so many sources of significant variance in the CHORS methodologies, that the HPLC system rarely operated within performance criteria capable of producing the requisite data quality. It is the recommendation of the investigative team to a) not correct the data, b) make all the data that was temporarily sequestered available for scientific use, and c) label the affected data with an appropriate warning, e.g., "These data are not validated and should not be used as the sole basis for a scientific result, conclusion, or hypothesis--independent corroborating evidence is required."

  13. The use of dihexyldithiocarbamate in reverse-phase HPLC of metal chelates

    Science.gov (United States)

    Fatimah, S. S.; Bahti, H. H.; Hastiawan, I.; Permanasari, A.

    2018-05-01

    Dialkyldithiocarbamates have long been used as chelating agents in reverse-phase HPLC of transition metals. In the previous study, an alkyl homolog of this type of ligand, namely dihexyldithiocarbamate (DHDTC), was synthesized and characterized. The use of this particular ligand in the revese-phase HPLC of some selected transition metal ions is now reported for the first time. The mobile phase comprising of the flow rate and of the detection, in the separation of the metal chelates of Cd (II), Fe (III), Cu (II), and Co (III), were investigated on a C-18 column. The results showed that dihexylditiocarbamate could be used for separating Cd (II), Fe(III), Cu(II), and Co(III). Therefore, it could be used in simultaneous analysis.

  14. Hepatocellular Carcinoma Metastasis to the Orbit in a Coinfected HIV+ HBV+ Patient Previously Treated with Orthotopic Liver Transplantation: A Case Report

    Directory of Open Access Journals (Sweden)

    S. Guerriero

    2011-01-01

    Full Text Available Hepatocellular carcinoma rarely metastasizes to the orbit. We report a 45-year-old male, HBV+, HIV+, with a past history of a liver transplant for ELSD (end-stage liver disease with hepatocellular carcinoma and recurrent HCC, who presented with proptosis and diplopia of the left eye. CT scans of the head revealed a large, irregular mass in the left orbit causing superior and lateral destruction of the orbital bone. Biopsy specimens of the orbital tumor showed features of metastatic foci of hepatocellular carcinoma. Only 16 other cases of HCC metastasis to the orbit have been described in literature, and this is the first case in a previously transplanted HIV+, HBV+ patient.

  15. Retinoid quantification by HPLC/MS(n)

    Science.gov (United States)

    McCaffery, Peter; Evans, James; Koul, Omanand; Volpert, Amy; Reid, Kevin; Ullman, M. David

    2002-01-01

    Retinoic acid (RA) mediates most of the biological effects of vitamin A that are essential for vertebrate survival. It acts through binding to receptors that belong to the nuclear receptor transcription factor superfamily (Mangelsdorf et al. 1994). It is also a highly potent vertebrate teratogen. To determine the function and effects of endogenous and exogenous RA, it is important to have a highly specific, sensitive, accurate, and precise analytical procedure. Current analyses of RA and other retinoids are labor intensive, of poor sensitivity, have limited specificity, or require compatibility with RA reporter cell lines (Chen et al. 1995. BIOCHEM: Pharmacol. 50: 1257-1264; Creech Kraft et al. 1994. BIOCHEM: J. 301: 111-119; Lanvers et al. 1996. J. Chromatogr. B Biomed. Appl. 685: 233-240; Maden et al. 1998. DEVELOPMENT: 125: 4133-4144; Wagner et al. 1992. DEVELOPMENT: 116: 55-66). This paper describes an HPLC/mass spectrometry/mass spectrometry product ion scan (HPLC/MS(n)) procedure for the analysis of retinoids that employs atmospheric pressure chemical ionization MS. The retinoids are separated by normal-phase column chromatography with a linear hexane-isopropanol-dioxane gradient. Each retinoid is detected by a unique series of MS(n) functions set at optimal collision-induced dissociation energy (30% to 32%) for all MS(n) steps. The scan events are divided into three segments, based on HPLC elution order, to maximize the mass spectrometer duty cycle. The all-trans, 9-cis, and 13-cis RA isomers are separated, if desired, by an isocratic hexane-dioxane-isopropanol mobile phase. This paper describes an HPLC/MS(n) procedure possessing high sensitivity and specificity for retinoids.

  16. Reverse Shoulder Arthroplasty for the Treatment of Rotator Cuff Deficiency: A Concise Follow-up, at a Minimum of 10 Years, of Previous Reports.

    Science.gov (United States)

    Cuff, Derek J; Pupello, Derek R; Santoni, Brandon G; Clark, Rachel E; Frankle, Mark A

    2017-11-15

    We previously evaluated 94 patients (96 shoulders) who underwent reverse shoulder arthroplasty using a central compressive screw with 5.0-mm peripheral locking screws for baseplate fixation and a center of rotation lateral to the glenoid as treatment for end-stage rotator cuff deficiency. The purpose of this study was to report updated results at a minimum follow-up of 10 years. Forty patients (42 shoulders) were available for clinical follow-up. In the patients available for study, implant survivorship, with the end point being revision for any reason, was 90.7%. Since our 5-year report, 2 patients underwent revision surgery; 1 patient sustained a periprosthetic fracture 7 years postoperatively and 1 patient had a dislocation because of chronic shoulder instability at 8 years postoperatively. At a minimum follow-up of 10 years, the patients continued to maintain their improved outcome scores and range of motion, which were comparable with earlier follow-up evaluations. Therapeutic Level IV. See Instructions for Authors for a complete description of levels of evidence.

  17. Case report of right hamate hook fracture in a patient with previous fracture history of left hamate hook: is it hamate bipartite?

    Directory of Open Access Journals (Sweden)

    Norton Sandra

    2006-10-01

    Full Text Available Abstract Background Hamate hook fracture is a common fracture in golfers and others who play sports that involve rackets or sticks such as tennis or hockey. This patient had a previous hamate fracture in the opposing wrist along with potential features of hamate bipartite. Case presentation A 19 year old male presented with a complaint of right wrist pain on the ulnar side of the wrist with no apparent mechanism of injury. The pain came on gradually one week before being seen in the office and he reported no prior care for the complaint. His history includes traumatic left hamate hook fracture with surgical excision. Conclusion The patient was found to have marked tenderness over the hamate and with a prior fracture to the other wrist, computed tomography of the wrist was ordered revealing a fracture to the hamate hook in the right wrist. He was referred for surgical evaluation and the hook of the hamate was excised. Post-surgically, the patient was able to return to normal activity within eight weeks. This case is indicative of fracture rather than hamate bipartite. This fracture should be considered in a case of ulnar sided wrist pain where marked tenderness is noted over the hamate, especially after participation in club or racket sports.

  18. Characterization of Cladosporols from the Marine Algal-Derived Endophytic Fungus Cladosporium cladosporioides EN-399 and Configurational Revision of the Previously Reported Cladosporol Derivatives.

    Science.gov (United States)

    Li, Hong-Lei; Li, Xiao-Ming; Mándi, Attila; Antus, Sándor; Li, Xin; Zhang, Peng; Liu, Yang; Kurtán, Tibor; Wang, Bin-Gui

    2017-10-06

    Four new cladosporol derivatives, cladosporols F-I (1-4), the known cladosporol C (5), and its new epimer, cladosporol J (6), were isolated and identified from the marine algal-derived endophytic fungus Cladosporium cladosporioides EN-399. Their structures were determined by detailed interpretation of NMR and MS data, and the absolute configurations were established on the basis of TDDFT-ECD and OR calculations. The configurational assignment of cladosporols F (1) and G (2) showed that the previously reported absolute configuration of cladosporol A and all the related cladosporols need to be revised from (4'R) to (4'S). Compounds 1-6 showed antibacterial activity against Escherichia coli, Micrococcus luteus, and Vibrio harveyi with MIC values ranging from 4 to 128 μg/mL. Compound 3 showed significant cytotoxicity against A549, Huh7, and LM3 cell lines with IC 50 values of 5.0, 1.0, and 4.1 μM, respectively, and compound 5 showed activity against H446 cell line with IC 50 value of 4.0 μM.

  19. Arrhythmias and sudden death among older children and young adults following tetralogy of Fallot repair in the current era: are previously reported risk factors still applicable?

    Science.gov (United States)

    Arya, Swati; Kovach, Julie; Singh, Harinder; Karpawich, Peter P

    2014-01-01

    Young adult patients (pts) with repaired tetralogy of Fallot (TOF) remain at risk for arrhythmias (Ar) and sudden cardiac death (SCD). Based on past studies with earlier pt subsets, Ar/SCD events were associated with right ventricular (RV) systolic pressures >60 mm Hg, outflow tract gradients >20 mm Hg, and QRS duration >180 ms. However, there are limited recent studies to evaluate these risk factors in the current patient generation. Patients with TOF followed over the past 50 years were grouped by presence of any arrhythmias (group 1), absence of arrhythmias (group 2), and presence of SCD or significant ventricular arrhythmias (group 3) and correlated with current pt age, gender, age at repair, repair types, echocardiogram, cardiac magnetic resonance imaging, electrocardiogram/Holter, hemodynamics, and electrophysiology findings. Of 109 pts, 52 were male aged 17-58 years. Of these, 59 (54%) had Ar, two of whom had SCD. These 59 pts were chronologically older at the time of analysis, with repair at an older age and wider QRS duration (78-240, mean 158 ms) when compared with those without Ar. However, there was no correlation with surgical era, surgical repair, gender, RV pressure >60 mm Hg, right ventricular outflow tract gradient >20 mm Hg, or RV end-diastolic volume on CMRI. Ar/SCD risk continues to correlate with repair age and advancing pt age. QRS duration is longer in these patients but at a shorter interval (mean 158 ms) and less RV pressure (mean 43 mm Hg) than previously reported. In the current TOF patient generation, neither surgical era, type of repair, RV outflow gradient nor RV volume correlate with Ar/SCD. Electrophysiologic testing to verify and identify arrhythmias remains clinically effective. © 2013 Wiley Periodicals, Inc.

  20. Structural analysis of eight novel and 112 previously reported missense mutations in the interactive FXI mutation database reveals new insight on FXI deficiency.

    Science.gov (United States)

    Saunders, Rebecca E; Shiltagh, Nuha; Gomez, Keith; Mellars, Gillian; Cooper, Carolyn; Perry, David J; Tuddenham, Edward G; Perkins, Stephen J

    2009-08-01

    Factor XI (FXI) functions in blood coagulation. FXI is composed of four apple (Ap) domains and a serine protease (SP) domain. Deficiency of FXI leads to an injury-related bleeding disorder, which is remarkable for the lack of correlation between bleeding symptoms and FXI coagulant activity (FXI:C). The number of mutations previously reported in our interactive web database (http://www.FactorXI.org) is now significantly increased to 183 through our new patient studies and from literature surveys. Eight novel missense mutations give a total of 120 throughout the FXI gene (F11). The most abundant defects in FXI are revealed to be those from low-protein plasma levels (Type I: CRM-) that originate from protein misfolding, rather than from functional defects (Type II: CRM+). A total of 70 Ap missense mutations were analysed using a consensus Ap domain structure generated from the FXI dimer crystal structure. This showed that all parts of the Ap domain were affected. The 47 SP missense mutations were also distributed throughout the SP domain structure. The periphery of the Ap beta-sheet structure is sensitive to structural perturbation caused by residue changes throughout the Ap domain, yet this beta-sheet is crucial for FXI dimer formation. Residues located at the Ap4:Ap4 interface in the dimer are much less directly involved. We conclude that the abundance of Type I defects in FXI results from the sensitivity of the Ap domain folding to residue changes within this, and discuss how structural knowledge of the mutations improves our understanding of FXI deficiencies.

  1. Literatuuronderzoek HPLC-methoden voor vitamine E

    OpenAIRE

    Altena, A.; Hollman, P.C.H.

    1985-01-01

    Doel van dit onderzoek is: het inventariseren van HPLC-methoden voor vitamine E, eventueel in combinatie met vitamine A, in levensmiddelen. Een overzicht van de in de literatuur beschreven HPLC-methoden vanaf ca. 1977 wordt gegeven.

  2. Determination of vitamins D2 and D3 in selected food matrices by online high-performance liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS).

    Science.gov (United States)

    Nestola, Marco; Thellmann, Andrea

    2015-01-01

    An online normal-phase liquid chromatography-gas chromatography-mass spectrometry (HPLC-GC-MS) method was developed for the determination of vitamins D2 and D3 in selected food matrices. Transfer of the sample from HPLC to GC was realized by large volume on-column injection; detection was performed with a time-of-flight mass spectrometer (TOF-MS). Typical GC problems in the determination of vitamin D such as sample degradation or sensitivity issues, previously reported in the literature, were not observed. Determination of total vitamin D content was done by quantitation of its pyro isomer based on an isotopically labelled internal standard (ISTD). Extracted ion traces of analyte and ISTD showed cross-contribution, but non-linearity of the calibration curve was not determined inside the chosen calibration range by selection of appropriate quantifier ions. Absolute limits of detection (LOD) and quantitation (LOQ) for vitamins D2 and D3 were calculated as approximately 50 and 150 pg, respectively. Repeatability with internal standard correction was below 2 %. Good agreement between quantitative results of an established high-performance liquid chromatography with UV detection (HPLC-UV) method and HPLC-GC-MS was found. Sterol-enriched margarine was subjected to HPLC-GC-MS and HPLC-MS/MS for comparison, because HPLC-UV showed strong matrix interferences. HPLC-GC-MS produced comparable results with less manual sample cleanup. In summary, online hyphenation of HPLC and GC allowed a minimization in manual sample preparation with an increase of sample throughput.

  3. HPLC-based quantification of bacterial housekeeping nucleotides and alarmone messengers ppGpp and pppGpp.

    Science.gov (United States)

    Varik, Vallo; Oliveira, Sofia Raquel Alves; Hauryliuk, Vasili; Tenson, Tanel

    2017-09-08

    Here we describe an HPLC-based method to quantify bacterial housekeeping nucleotides and the signaling messengers ppGpp and pppGpp. We have replicated and tested several previously reported HPLC-based approaches and assembled a method that can process 50 samples in three days, thus making kinetically resolved experiments feasible. The method combines cell harvesting by rapid filtration, followed by acid extraction, freeze-drying with chromatographic separation. We use a combination of C18 IPRP-HPLC (GMP unresolved and co-migrating with IMP; GDP and GTP; AMP, ADP and ATP; CTP; UTP) and SAX-HPLC in isocratic mode (ppGpp and pppGpp) with UV detection. The approach is applicable to bacteria without the requirement of metabolic labelling with 32P-labelled radioactive precursors. We applied our method to quantify nucleotide pools in Escherichia coli BW25113 K12-strain both throughout the growth curve and during acute stringent response induced by mupirocin. While ppGpp and pppGpp levels vary drastically (40- and ≥8-fold, respectively) these changes are decoupled from the quotients of the housekeeping pool and guanosine and adenosine housekeeping nucleotides: NTP/NDP/NMP ratio remains stable at 6/1/0.3 during both normal batch culture growth and upon acute amino acid starvation.

  4. A diagnostic dilemma: Left-sided appendicitis in a 10 year old boy with previously undiagnosed intestinal malrotation. A case report

    Directory of Open Access Journals (Sweden)

    Ashvini Shekhar

    2015-01-01

    Conclusion: Left sided acute appendicitis is a diagnostic dilemma, thus often leading to management delays. It is pertinent to remember that malrotation of the gut is more common than previously thought, and not just a disease of infancy. It is advisable to consider imaging studies while balancing the risk-benefit-ratio of radiation exposure, especially in paediatric cases to cinch the diagnosis.

  5. Laparoscopy After Previous Laparotomy

    Directory of Open Access Journals (Sweden)

    Zulfo Godinjak

    2006-11-01

    Full Text Available Following the abdominal surgery, extensive adhesions often occur and they can cause difficulties during laparoscopic operations. However, previous laparotomy is not considered to be a contraindication for laparoscopy. The aim of this study is to present that an insertion of Veres needle in the region of umbilicus is a safe method for creating a pneumoperitoneum for laparoscopic operations after previous laparotomy. In the last three years, we have performed 144 laparoscopic operations in patients that previously underwent one or two laparotomies. Pathology of digestive system, genital organs, Cesarean Section or abdominal war injuries were the most common causes of previouslaparotomy. During those operations or during entering into abdominal cavity we have not experienced any complications, while in 7 patients we performed conversion to laparotomy following the diagnostic laparoscopy. In all patients an insertion of Veres needle and trocar insertion in the umbilical region was performed, namely a technique of closed laparoscopy. Not even in one patient adhesions in the region of umbilicus were found, and no abdominal organs were injured.

  6. Separation, purification and identification of flavonoid glycosides using reversed phase hplc

    International Nuclear Information System (INIS)

    Hasan, A.; Khan, M.A.

    2002-01-01

    Optimal high performance liquid chromatography (HPLC) separation conditions and semi-preparative scale isolation of flavonoid glycosides from three plant species namely Vitex nagunda, Rubus ulmifolious and Malotus philipensis is reported. Identification of purified flavonoid glycoside was achieved using spiking technique in HPLC. (author)

  7. Exorphin Peptides in Urine with HPLC-MS/MS Detection

    OpenAIRE

    2015-01-01

    Exorphins have been found in urine from individuals diagnosed with autism spectrum disorders by HPLC techniques. However, several studies, using sophisticated analytical techniques , have reported negative findings. This made it necessary to improve our methods. The sample stability during transport and storage and the pre -analytical treatment of urines was improved by peptidase inhibition and solid ...

  8. De novo adamantinomatous craniopharyngioma presenting anew in an elderly patient with previous normal CT and MRI studies: A case report and implications on pathogenesis

    Directory of Open Access Journals (Sweden)

    Amy Walker, B.S.

    2015-09-01

    Full Text Available Adamantinomatous craniopharyngiomas are histologically benign epithelial tumors which arise from embryonic remnants of the craniopharyngeal duct and Rathke’s pouch. They are thought to have a congenital origin and are histologically unique from papillary craniopharyngioma. We describe the case of an elderly male who presented with symptoms related to a large craniopharyngioma with previously normal brain magnetic resonance and computed tomography imaging studies. These findings dispute the embryogenic theory that craniopharyngiomas observed in adults develop from the persistent slow growth of embryonic remnants.

  9. Application of the electromagnetic borehole flowmeter and evaluation of previous pumping tests at Paducah Gaseous Diffusion Plant. Final report, June 15, 1992--August 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Young, S.C.; Julian, S.C.; Neton, M.J.

    1993-01-01

    Multi-well pumping tests have been concluded at wells MW79, MW108, and PW1 at the Paducah Gaseous Diffusion Plant (PGDP) to determine the hydraulic properties of the Regional Gravel Aquifer (RGA). Soil cores suggest that the RGA consists of a thin sandy facies (2 to 6 feet) at the top of a thicker (> 10 feet) gravelly facies. Previous analyses have not considered any permeability contrast between the two facies. To assess the accuracy of this assumption, TVA personnel conducted borehole flowmeter tests at wells MW108 and PW1. Well MW79 could not be tested. The high K sand unit is probably 10 times more permeable than comparable zone in the gravelly portion of the RGA. Previous analyses of the three multi-well aquifer tests do not use the same conceptual aquifer model. Data analysis for one pumping test assumed that leakance was significant. Data analysis for another pumping test assumed that a geologic boundary was significant. By collectively analyzing all three tests with the borehole flowmeter results, the inconsistency among the three pumping tests can be explained. Disparity exists because each pumping test had a different placement of observation wells relative to the high K zone delineating by flowmeter testing.

  10. Previous ISD Program Review.

    Science.gov (United States)

    1981-03-01

    report. The detail required for such a review would be unwieldy and would comsume inordinate amounts of time. The result of the document review will...attempts have been made at writing specific behavioral objectives (SBOs). These, however, have proven to be inadequate in that they are not stated in... behavioral terms (e.g., "will understand," "will have a knowledge of," etc.). C. Development of CRO/CRTs? In nearly all cases, ISD teams are just

  11. Two case reports: Carcinoma of the cervix and carcinoma of the endometrium treated with radiotherapy after previous irradiation for benign uterine bleeding

    Energy Technology Data Exchange (ETDEWEB)

    MacLeod, C. [Royal Prince Alfred Hospital, Camperdown, NSW (Australia). Department of Radiation Oncology

    1998-08-01

    In the 1940s, 1950s and 1960s, low doses of radiotherapy were used to treat benign uterine bleeding. The cases of two women who received this form of therapy and later developed gynaecological malignancies and had high-dose pelvic radiotherapy are presented. A 76-year-old woman with an International Federation of Gynecology and Obstetrics (FIGO) stage-II B squamous cell carcinoma of the cervix received external beam radiotherapy and intra-uterine brachytherapy and a 77-year-old woman with a FIGO stage-I B endometrial adenocarcinoma received adjuvant postoperative pelvic radiotherapy. Both women had a significant past history of low-dose-rate intra-uterine irradiation for dysfunctional uterine bleeding. Therefore the theoretical question of carcinogenesis was raised, and also the practical questions of what dose had previously been given and what further dose could be safely given with regard to normal tissue tolerance. Copyright (1998) Blackwell Science Pty Ltd 20 refs.

  12. Two case reports: Carcinoma of the cervix and carcinoma of the endometrium treated with radiotherapy after previous irradiation for benign uterine bleeding

    International Nuclear Information System (INIS)

    MacLeod, C.

    1998-01-01

    In the 1940s, 1950s and 1960s, low doses of radiotherapy were used to treat benign uterine bleeding. The cases of two women who received this form of therapy and later developed gynaecological malignancies and had high-dose pelvic radiotherapy are presented. A 76-year-old woman with an International Federation of Gynecology and Obstetrics (FIGO) stage-II B squamous cell carcinoma of the cervix received external beam radiotherapy and intra-uterine brachytherapy and a 77-year-old woman with a FIGO stage-I B endometrial adenocarcinoma received adjuvant postoperative pelvic radiotherapy. Both women had a significant past history of low-dose-rate intra-uterine irradiation for dysfunctional uterine bleeding. Therefore the theoretical question of carcinogenesis was raised, and also the practical questions of what dose had previously been given and what further dose could be safely given with regard to normal tissue tolerance. Copyright (1998) Blackwell Science Pty Ltd

  13. The use of porcine small intestinal submucosa mesh (SURGISIS as a pelvic sling in a man and a woman with previous pelvic surgery: two case reports

    Directory of Open Access Journals (Sweden)

    Al-Sahaf Osama

    2009-02-01

    Full Text Available Abstract Introduction Closing the pelvic peritoneum to prevent the small bowel dropping into the pelvis after surgery for locally recurrent rectal cancer is important to prevent adhesions deep in the pelvis or complications of adjuvant radiotherapy. Achieving this could be difficult because sufficient native tissue is unavailable; we report on the use of small intestine submucosa extra-cellular matrix mesh in the obliteration of the pelvic brim. Case presentation We describe two cases in which submucosa extra-cellular matrix mesh was used to obliterate the pelvic brim following resection of a recurrent rectal tumour; the first patient, a 78-year-old Caucasian man, presented with small bowel obstruction caused by adhesions to a recurrent rectal tumour. The second patient, an 84-year-old Caucasian woman, presented with vaginal discharge caused by an entero-vaginal fistula due to a recurrent rectal tumour. Conclusion We report on the use of submucosa extra-cellular matrix mesh as a pelvic sling in cases where primary closure of the pelvic peritoneum is unfeasible. Its use had no infective complications and added minimal morbidity to the postoperative period. This is an original case report that would be of interest to general and colorectal surgeons.

  14. "Salting-out" concentration of phytoplankton pigment extracts previous to their analysis by HPLC

    Directory of Open Access Journals (Sweden)

    José Luis Garrido

    2014-04-01

    The recoveries of different pigments varied depending on their chemical nature and the degree of enrichment of the extract. Carotenoids and non-polar chlorophylls were recovered above 85 % with 5M saline solutions, while the recovery of acidic clorophylls (c3 and c2 decreased with enrichment factors.

  15. Four Forensic Entomology Case Studies: Records and Behavioral Observations on Seldom Reported Cadaver Fauna With Notes on Relevant Previous Occurrences and Ecology.

    Science.gov (United States)

    Lindgren, Natalie K; Sisson, Melissa S; Archambeault, Alan D; Rahlwes, Brent C; Willett, James R; Bucheli, Sibyl R

    2015-03-01

    A yearlong survey of insect taxa associated with human decomposition was conducted at the Southeast Texas Applied Forensic Science (STAFS) facility located in the Center for Biological Field Studies of Sam Houston State University in Huntsville, TX. During this study, four insect-cadaver interactions were observed that represent previously poorly documented yet forensically significant interactions: Syrphidae maggots colonized a corpse in an aquatic situation; Psychodidae adults mated and oviposited on an algal film that was present on a corpse that had been recently removed from water; several Panorpidae were the first insects to feed upon a freshly placed corpse in the autumn; and a noctuid caterpillar was found chewing and ingesting dried human skin. Baseline knowledge of insect-cadaver interactions is the foundation of forensic entomology, and unique observations have the potential to expand our understanding of decomposition ecology. © The Author 2015. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

  16. Homozygous loss of function BRCA1 variant causing a Fanconi-anemia-like phenotype, a clinical report and review of previous patients.

    Science.gov (United States)

    Freire, Bruna L; Homma, Thais K; Funari, Mariana F A; Lerario, Antônio M; Leal, Aline M; Velloso, Elvira D R P; Malaquias, Alexsandra C; Jorge, Alexander A L

    2018-03-01

    Fanconi Anemia (FA) is a rare and heterogeneous genetic syndrome. It is associated with short stature, bone marrow failure, high predisposition to cancer, microcephaly and congenital malformation. Many genes have been associated with FA. Previously, two adult patients with biallelic pathogenic variant in Breast Cancer 1 gene (BRCA1) had been identified in Fanconi Anemia-like condition. The proband was a 2.5 year-old girl with severe short stature, microcephaly, neurodevelopmental delay, congenital heart disease and dysmorphic features. Her parents were third degree cousins. Routine screening tests for short stature was normal. We conducted whole exome sequencing (WES) of the proband and used an analysis pipeline to identify rare nonsynonymous genetic variants that cause short stature. We identified a homozygous loss-of-function BRCA1 mutation (c.2709T > A; p. Cys903*), which promotes the loss of critical domains of the protein. Cytogenetic study with DEB showed an increased chromosomal breakage. We screened heterozygous parents of the index case for cancer and we detected, in her mother, a metastatic adenocarcinoma in an axillar lymph node with probable primary site in the breast. It is possible to consolidate the FA-like phenotype associated with biallelic loss-of-function BRCA1, characterized by microcephaly, short stature, developmental delay, dysmorphic face features and cancer predisposition. In our case, the WES allowed to establish the genetic cause of short stature in the context of a chromosome instability syndrome. An identification of BRCA1 mutations in our patient allowed precise genetic counseling and also triggered cancer screening for the patient and her family members. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  17. Feline leprosy due to Candidatus 'Mycobacterium lepraefelis': Further clinical and molecular characterisation of eight previously reported cases and an additional 30 cases.

    Science.gov (United States)

    O'Brien, Carolyn R; Malik, Richard; Globan, Maria; Reppas, George; McCowan, Christina; Fyfe, Janet A

    2017-09-01

    This paper, the last in a series of three on 'feline leprosy', provides a detailed description of disease referable to the previously unnamed species, Candidatus 'Mycobacterium lepraefelis', a close relative of the human pathogens Mycobacterium leprae and Mycobacterium lepromatosis. Cases were sourced retrospectively and prospectively for this observational study, describing clinical, geographical and molecular microbiological data for cats definitively diagnosed with Candidatus 'M lepraefelis' infection. A total of 145 cases of feline leprosy were scrutinised; 114 'new' cases were sourced from the Victorian Infectious Diseases Reference Laboratory (VIDRL) records, veterinary pathology laboratories or veterinarians, and 31 cases were derived from six published studies. Thirty-eight cats were definitively diagnosed with Candidatus 'M lepraefelis' infection. Typically, cats tended to be middle-aged or older when first infected, with a male predilection. Affected cats typically had widespread cutaneous lesions, in some cases after initially localised disease. Advanced cases were often systemically unwell. All cats had outdoor access. The histological picture was lepromatous in the majority of patients, although two cases had tuberculoid disease. In one case that underwent necropsy, lesions were evident in the liver, spleen and lungs. Treatment was varied, although most cats received a combination of oral clarithromycin and rifampicin. Prognosis for recovery was variable, but typically poor. Candidatus 'M lepraefelis' typically causes high bacterial index (lepromatous) feline leprosy that in some cases progresses to systemic mycobacteriosis. The disease has a variable clinical course and prognosis. Many cases either died or were euthanased due to the infection. Multilocus sequence analysis reveals a heterogeneous picture and further analysis of draft genome sequencing may give clues to the taxonomy and epidemiology of this organism. Prospective treatment trials and

  18. Majewski osteodysplastic primordial dwarfism type II (MOPD II) syndrome previously diagnosed as Seckel syndrome: report of a novel mutation of the PCNT gene.

    Science.gov (United States)

    Piane, Maria; Della Monica, Matteo; Piatelli, Gianluca; Lulli, Patrizia; Lonardo, Fortunato; Chessa, Luciana; Scarano, Gioacchino

    2009-11-01

    We report on a 3-year-old boy with prenatal onset of proportionate dwarfism, postnatal severe microcephaly, high forehead with receded hairline, sparse scalp hair, beaked nose, mild retrognathia and hypotonia diagnosed at birth as Seckel syndrome. At age 3 years, he became paralyzed due to a cerebrovascular malformation. Based on the clinical and radiological features showing evidence of skeletal dysplasia, the diagnosis was revised to Majewski osteodysplastic primordial dwarfism type II (MOPD II) syndrome. Western blot analysis of the patient's lymphoblastoid cell line lysate showed the absence of the protein pericentrin. Subsequent molecular analysis identified a novel homozygous single base insertion (c.1527_1528insA) in exon 10 of the PCNT gene, which leads to a frameshift (Treo510fs) and to premature protein truncation. PCNT mutations must be considered diagnostic of MOPD II syndrome. A possible role of pericentrin in the development of cerebral vessels is suggested. Copyright 2009 Wiley-Liss, Inc.

  19. Radiation port cutaneous metastases: Reports of two patients whose recurrent visceral cancers presented as skin lesions at the site of previous radiation and literature review

    Directory of Open Access Journals (Sweden)

    Brian Spencer Hoyt

    2014-01-01

    Full Text Available Radiation therapy is associated with a variety of complications, including the development of primary skin cancers in the radiated region. However, it is rare for patients with visceral cancers who are treated with radiation therapy to subsequently develop cutaneous metastasis within the radiation port. We describe two patients with internal malignancies who developed cutaneous metastases within their radiation ports following radiotherapy. In addition, we used PubMed to perform an extensive literature review and identify additional reports of cutaneous metastasis within a radiation port. We excluded patients who developed melanoma or primary skin cancers in the radiation port. We also excluded patients with non-solid organ malignancies. Herein, we summarize the characteristics of 23 additional patients who experienced radiation port cutaneous metastases and explore possible mechanisms for the occurrence of radiation port cutaneous metastases.

  20. Late type III endoleak after thoracic endovascular aneurysm repair and previous infrarenal stent graft implantation - a case report and review of the literature.

    Science.gov (United States)

    Leszczyński, Jerzy; Macioch, Waldemar; Chudziński, Witold; Gałązka, Zbigniew

    2017-09-01

    Thoracic endovascular aortic repair (TEVAR) effectively improved the results of thoracic aortic aneurysm treatment. TEVAR is a less invasive procedure that can be performed under local anesthesia with shorter hospital stay. The perioperative morbidity and mortality rates are lower for endovascular than open repair, but the rate of secondary interventions is higher for TEVAR. We report a case of an elderly man with synchronous abdominal and thoracic aortic aneurysms. A type III dangerous endoleak was recognized 3 years after TEVAR. It was successfully repaired during an endovascular procedure. There were no new endoleaks after 12 months of follow-up. TEVAR may be the only option of treatment for risky and elderly patients. However, postoperative monitoring is necessary to exclude different types of endoleaks. Most of them undergo effective endovascular repair.

  1. Resolution of temporomandibular joint dysfunction (TMJD) by correcting a lateral head translation posture following previous failed traditional chiropractic therapy: a CBP® case report.

    Science.gov (United States)

    Jaeger, Jason O; Oakley, Paul A; Moore, Robert R; Ruggeroli, Edward P; Harrison, Deed E

    2018-01-01

    [Purpose] To present the case of the resolution of right temporomandibular joint dysfunction (TMJD) following the correction of a right lateral head translation posture. [Subject and Methods] A 24 year old female reported facial pain and jaw clicking in the right TMJ. Radiography revealed a 19 mm right head (shift) translation posture. TMJ vibration analysis showed characteristic abnormalities for the right TMJ. The patient was treated with CBP ® technique mirror image ® left sided exercises, and traction methods as well as spinal manipulative therapy (SMT). [Results] After 36 treatments over a 12-week time period, a complete correction of the lateral head posture was achieved corresponding with a complete resolution of jaw pain and clicking. TMJ vibration analysis demonstrated normal right side TMJ characteristics following treatment. [Conclusion] Abnormal head/neck postures, such as lateral head translation, may be an unrealized source of TMJD and may be explained through the 'regional interdependence' model or by how seemingly unrelated anatomy may be associated with a primary complaint.

  2. HPLC ‘Multi-Analyte’ Detection Method

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    The application of multi-analyte methods for pesticides carrying chromophoric structures by HPLC is described. Details are given on the materials and methods used. Recorded UV spectra of active substances are presented for allowing the verification of purity and the confirmation of substances eluting from the HPLC column. (author)

  3. Quality Control of Selected Pesticides with HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Karasali, H. [Benaki Phytopathological Institute Laboratory of Physical and Chemical Analysis of Pesticides, Ekalis (Greece)

    2009-07-15

    Laboratory data obtained on two different HPLC separation columns and detection by UV and DAD under repeatability conditions are presented and discussed. The behaviour of pesticides on different HPLC columns under gradient and isocratic conditions is evaluated concerning the applicability of respective methodologies. Representative chromatograms of real formulations and “empty” formlants are given for illustration. (author)

  4. HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication

    DEFF Research Database (Denmark)

    Johansen, Kenneth; Wubshet, Sileshi Gizachew; Nyberg, Nils

    2013-01-01

    Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC......–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts......, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin...

  5. Measurements of urinary kinins by HPLC-radioimmunoassay

    International Nuclear Information System (INIS)

    Fejes-Toth, G.; Naray-Fejes-Toth, A.; Froelich, J.C.

    1984-01-01

    In this paper the authors describe a method for the individual determination of urinary kinins. Extraction from the urine is performed on an Amberlite CG-50 column and kinins are eluted with formic acid. The samples are further purified and kinins are separated by reversed phase HPLC. Bradykinin and lysylbradykinin are quantified by a sensitive radioimmunoassay capable of detecting 0.1 fmol of either peptide. Procedural losses are monitored by measuring the recovery of [ 3 H]bradykinin and [ 3 H]lysylbradykinin. Simple methods for labeling of bradykinin and lysylbradykinin with tritium are also presented. Recoveries of [ 3 H]bradykinin and [ 3 H]lysylbradykinin from biological material ranged between 77 and 91%. The combination of HPLC with radioimmunoassay makes it possible to determine kinin concentrations of biological samples with a higher sensitivity and greater specificity than previous methods. (Auth.)

  6. INTRODUCTION Previous reports have documented a high ...

    African Journals Online (AJOL)

    Conclusion: The positive effect of education on oral hygiene practices is highlighted in this study. However there is still need for proper health enlightenment in this population with regards to use of the available oral health care facilities. Keywords: Oral hygiene, Pregnancy, Nigeria. Annals of Ibadan Postgraduate Medicine.

  7. Femoral Component Revision with Use of Impaction Bone-Grafting and a Cemented Polished Stem: A Concise Follow-up, at Fifteen to Twenty Years, of a Previous Report*

    NARCIS (Netherlands)

    Te Stroet, M.A.; Gardeniers, J.W.M.; Verdonschot, N.J.; Rijnen, W.H.C.; Slooff, T.J.J.H.; Schreurs, B.W.

    2012-01-01

    We previously reported our results for thirty-three consecutive femoral component revisions with impaction bone-grafting, performed with the X-change femoral revision system and a cemented polished Exeter stem, at a minimum of eight years of follow-up. The present updated study shows the results

  8. HPLC for quality control of polyimides

    Science.gov (United States)

    Young, P. R.; Sykes, G. F.

    1979-01-01

    High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

  9. Expermental Studies of quantitative evaluation using HPLC

    Directory of Open Access Journals (Sweden)

    Ki Rok Kwon

    2005-06-01

    Full Text Available Methods : This study was conducted to carry out quantitative evaluation using HPLC Content analysis was done using HPLC Results : According to HPLC analysis, each BVA-1 contained approximately 0.36㎍ melittin, and BVA-2 contained approximately 0.54㎍ melittin. But the volume of coating was so minute, slight difference exists between each needle. Conclusion : Above results indicate that the bee venom acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

  10. HPLC-Based Method to Evaluate Kinetics of Glucosinolate Hydrolysis by Sinapis alba Myrosinase1

    Science.gov (United States)

    Vastenhout, Kayla J.; Tornberg, Ruthellen H.; Johnson, Amanda L.; Amolins, Michael W.; Mays, Jared R.

    2014-01-01

    Isothiocyanates (ITCs) are one of several hydrolysis products of glucosinolates, plant secondary metabolites which are substrates for the thioglucohydrolase myrosinase. Recent pursuits toward the development of synthetic, non-natural ITCs have consequently led to an exploration of generating these compounds from non-natural glucosinolate precursors. Evaluation of the myrosinase-dependent conversion of select non-natural glucosinolates to non-natural ITCs cannot be accomplished using established UV-Vis spectroscopic methods. To overcome this limitation, an alternative HPLC-based analytical approach was developed where initial reaction velocities were generated from non-linear reaction progress curves. Validation of this HPLC method was accomplished through parallel evaluation of three glucosinolates with UV-Vis methodology. The results of this study demonstrate that kinetic data is consistent between both analytical methods and that the tested glucosinolates respond similarly to both Michaelis–Menten and specific activity analyses. Consequently, this work resulted in the complete kinetic characterization of three glucosinolates with Sinapis alba myrosinase, with results that were consistent with previous reports. PMID:25068719

  11. 72 - 80_Aminu_HPLC1

    African Journals Online (AJOL)

    pc

    HPLC, Gymnema sylvestre, carbohydrate hydrolyzing enzymes, lipid a chronic .... Method. Test for Tannins and Flavonoids was by. Trease and Evans (2002). Soluble Starch ... Fenton reaction was quantified using 2- deoxyribose oxidative ...

  12. Iridoids as chemical markers of false ipecac (Ronabea emetica), a previously confused medicinal plant.

    Science.gov (United States)

    Berger, Andreas; Fasshuber, Hannes; Schinnerl, Johann; Robien, Wolfgang; Brecker, Lothar; Valant-Vetschera, Karin

    2011-12-08

    Several roots or rhizomes of rubiaceous species are reportedly used as the emetic and antiamoebic drug ipecac. True ipecac (Carapichea ipecacuanha) is chemically well characterized, in contrast to striated or false ipecac derived from the rhizomes of Ronabea emetica (syn. Psychotria emetica). Besides its previous use as substitute of ipecac, the latter species is applied in traditional medicine of Panama and fruits of its relative Ronabea latifolia are reported as curare additives from Colombia. Compounds of Ronabea emetica were isolated using standard chromatographic techniques, and structurally characterized by NMR spectroscopy and mass spectrometry. Organ specific distribution in Ronabea emetica as well as in Ronabea latifolia was further assessed by comparative HPLC analysis. Four iridoid-glucosides, asperuloside (1), 6α-hydroxygeniposide (2), deacetylasperulosidic acid (3) and asperulosidic acid (4) were extracted from leaves of Ronabea emetica. Rhizomes, used in traditional medicine, were dominated by 3. HPLC profiles of Ronabea latifolia were largely corresponding. These results contrast to the general tendency of producing emetine-type and indole alkaloids in species of Psychotria and closely related genera and merit chemotaxonomic significance, characterizing the newly delimited genus Ronabea. The aim of the work was to resolve the historic problem of adulteration of ipecac by establishing the chemical profile of Ronabea emetica, the false ipecac, as one of its less known sources. The paper demonstrates that different sources of ipecac can be distinguished by their phytochemistry, thus contributing to identifying adulterations of true ipecac. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  13. Improved HPLC assay for S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721) in plasma

    International Nuclear Information System (INIS)

    Swynnerton, N.F.; McGovern, E.P.; Nino, J.A.; Mangold, D.J.

    1984-01-01

    An HPLC assay is presented for the detection and quantitation of the radioprotective drug S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721, ethiofos) present in plasma. Improved selectivity and a 40-fold increase in sensitivity have been demonstrated over the method previously reported by this laboratory. Using precolumn derivatization with fluorescamine and S-3-(4-aminobutylamino)propyl phosphorothioate (WR-80855, a homolog of WR-2721) as the internal standard, drug levels of 0.05 to 1000 μg/mL were determined with excellent precision. Detector response was linear over the entire range. The assay uses 150 μL of plasma and requires a total chromatography time of about 50 minutes. The method was found suitable for pharmacokinetic studies in a preliminary experiment with a beagle dog in which no interferences due to plasma constituents or drug metabolites were observed

  14. Characterization of primary standards for use in the HPLC analysis of the procyanidin content of cocoa and chocolate containing products.

    Science.gov (United States)

    Hurst, William J; Stanley, Bruce; Glinski, Jan A; Davey, Matthew; Payne, Mark J; Stuart, David A

    2009-10-15

    This report describes the characterization of a series of commercially available procyanidin standards ranging from dimers DP = 2 to decamers DP = 10 for the determination of procyanidins from cocoa and chocolate. Using a combination of HPLC with fluorescence detection and MALDI-TOF mass spectrometry, the purity of each standard was determined and these data were used to determine relative response factors. These response factors were compared with other response factors obtained from published methods. Data comparing the procyanidin analysis of a commercially available US dark chocolate calculated using each of the calibration methods indicates divergent results and demonstrate that previous methods may significantly underreport the procyanidins in cocoa-containing products. These results have far reaching implications because the previous calibration methods have been used to develop data for a variety of scientific reports, including food databases and clinical studies.

  15. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    Energy Technology Data Exchange (ETDEWEB)

    Hong, L; Altorfer, H R [Institute of Pharmaceutical Science, Swiss Federal Institute of Technology (ETH), Zurich (Switzerland); Horni, A; Hesse, M [Institute of Organic Chemistry, University of Zurich, Zurich (Switzerland)

    2005-07-01

    The radiolysis products of chloramphenicol under {gamma}-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of {gamma}-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by {gamma}-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  16. Identification and evaluation of radiolysis products of irradiated chloramphenicol by HPLC-MS and HPLC-DAD

    International Nuclear Information System (INIS)

    Hong, L.; Altorfer, H.R.; Horni, A.; Hesse, M.

    2005-01-01

    The radiolysis products of chloramphenicol under γ-radiation sterilization were investigated systematically in the present study. Eight main radiolysis products were identified and quantified by HPLC-MS and HPLC-DAD, including two compounds that have never been reported. The minor radiolysis products were quantified, which shows that they are at the concentration levels below the threshold for identification. Carbon-carbon rupture reaction and oxidation reaction were proposed as the main radiolysis reactions of chloramphenicol powder. The applicability of γ-sterilization for chloramphenicol products was quantitatively evaluated with qualitative and quantitative data and the data were compared to the threshold requirements of international regulations for identification. It was concluded that toxicities of the radiolysis products of chloramphenicol produced by γ-radiation sterilization can be neglected, the radiolysis products are safe for human health from chemical view. (author)

  17. HPLC-MS and GC-MS analyses combined with orthogonal partial least squares to identify cytotoxic constituents from turmeric (Curcuma longa L.).

    Science.gov (United States)

    Jiang, Jianlan; Zhang, Huan; Li, Zidan; Zhang, Xiaohang; Su, Xin; Li, Yan; Qiao, Bin; Yuan, Yingjin

    2013-08-01

    We investigated the fingerprints of 48 batches of turmeric total extracts (TTE) by HPLC-MS-MS and GC-MS analyses and 43 characteristic peaks (22 constituents from HPLC-MS-MS; 21 from GC-MS) were analyzed qualitatively and quantitatively. An MTT {3-(4,5-dimethylthiazol-2-yl)- 2,5-diphenyltetrazolium bromide} assay was implemented to measure the cytotoxicity of the TTE against HeLa cells. Then we utilized orthogonal partial least squares analysis, which correlated the chemical composition of the TTE to its cytotoxic activity, to identify potential cytotoxic constituents from turmeric. The result showed that 19 constituents contributed significantly to the cytotoxicity. The obtained result was verified by canonical correlation analysis. Comparison with previous reports also indicated some interaction between the curcuminoids and sesquiterpenoids in turmeric.

  18. Rapid HPLC-MS method for the simultaneous determination of tea catechins and folates.

    Science.gov (United States)

    Araya-Farias, Monica; Gaudreau, Alain; Rozoy, Elodie; Bazinet, Laurent

    2014-05-14

    An effective and rapid HPLC-MS method for the simultaneous separation of the eight most abundant tea catechins, gallic acid, and caffeine was developed. These compounds were rapidly separated within 9 min by a linear gradient elution using a Zorbax SB-C18 packed with sub 2 μm particles. This methodology did not require preparative and semipreparative HPLC steps. In fact, diluted tea samples can be easily analyzed using HPLC-MS as described in this study. The use of mass spectrometry detection for quantification of catechins ensured a higher specificity of the method. The percent relative standard deviation was generally lower than 4 and 7% for most of the compounds tested in tea drinks and tea extracts, respectively. Furthermore, the method provided excellent resolution for folate determination alone or in combination with catechins. To date, no HPLC method able to discriminate catechins and folates in a quick analysis has been reported in the literature.

  19. Chemical Differentiation of Dendrobium officinale and Dendrobium devonianum by Using HPLC Fingerprints, HPLC-ESI-MS, and HPTLC Analyses

    Science.gov (United States)

    Ye, Zi; Dai, Jia-Rong; Zhang, Cheng-Gang; Lu, Ye; Wu, Lei-Lei; Gong, Amy G. W.; Wang, Zheng-Tao

    2017-01-01

    The stems of Dendrobium officinale Kimura et Migo (Dendrobii Officinalis Caulis) have a high medicinal value as a traditional Chinese medicine (TCM). Because of the limited supply, D. officinale is a high priced TCM, and therefore adulterants are commonly found in the herbal market. The dried stems of a closely related Dendrobium species, Dendrobium devonianum Paxt., are commonly used as the substitute; however, there is no effective method to distinguish the two Dendrobium species. Here, a high performance liquid chromatography (HPLC) method was successfully developed and applied to differentiate D. officinale and D. devonianum by comparing the chromatograms according to the characteristic peaks. A HPLC coupled with electrospray ionization multistage mass spectrometry (HPLC-ESI-MS) method was further applied for structural elucidation of 15 flavonoids, 5 phenolic acids, and 1 lignan in D. officinale. Among these flavonoids, 4 flavonoid C-glycosides were firstly reported in D. officinale, and violanthin and isoviolanthin were identified to be specific for D. officinale compared with D. devonianum. Then, two representative components were used as chemical markers. A rapid and reliable high performance thin layer chromatography (HPTLC) method was applied in distinguishing D. officinale from D. devonianum. The results of this work have demonstrated that these developed analytical methods can be used to discriminate D. officinale and D. devonianum effectively and conveniently. PMID:28769988

  20. High performance liquid chromatography (HPLC fingerprints and primary structure identification of corn peptides by HPLC-diode array detection and HPLC-electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Chi Wang

    2016-01-01

    Full Text Available Corn peptides (CPs are reported to have many biological functions, such as facilitating alcohol metabolism, antioxidation, antitumor, antihypertension, and hepatoprotection. To develop a method for quality control, the high-performance liquid chromatography (HPLC system was applied. Twenty-eight common peaks were found in all the CPs of corn samples from Enshi, China, based on which, a fingerprinting chromatogram was established for use in quality control in future research. Subsequently, the major chemical constituents of these common peaks were identified respectively using the HPLC-diode-array detection electrospray ionization tandem mass spectrometry (DAD-ESI-MS/MS system, and 48 peptide fractions were determined ultimately. This was the first time for the majority of these peptides to be reported, and many of them contained amino acids of glutamine (Q, L and A, which might play an important role in the exhibition of the bioactivities of CPs. Many peptides had a similar primary structure to the peptides which had been proven to be bioactive such as facilitating alcohol metabolism, scavenging free radicals, and inhibiting lipid peroxidation. This systematical analysis of the primary structure of CPs facilitated subsequent studies on the relationship between the structures and functions, and could accelerate holistic research on CPs.

  1. Methods and applications of HPLC-AMS

    International Nuclear Information System (INIS)

    Buchholz, Bruce A.; Dueker, Stephen R.; Lin, Yumei; Clifford, Andrew J.; Vogel, John S.

    2000-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a 14 C-labeled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the 14 C content above the control predose tissue and converting to equivalents of the parent compound. High performance liquid chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are tentatively identified by co-elution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the 14 C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of 14 C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected 14 C activity <0.17 Bq (4.5 pCi) on the HPLC column

  2. An Inexpensive Digital Gradient Controller for HPLC.

    Science.gov (United States)

    Brady, James E.; Carr, Peter W.

    1983-01-01

    Use of gradient elution techniques in high performance liquid chromatography (HPLC) is often essential for direct separation of complex mixtures. Since most commercial controllers have features that are of marginal value for instructional purposes, a low-cost controller capable of illustrating essential features of gradient elution was developed.…

  3. HIV risk perception and testing behaviours among men having sex with men (MSM) reporting potential transmission risks in the previous 12 months from a large online sample of MSM living in Germany.

    Science.gov (United States)

    Marcus, Ulrich; Gassowski, Martyna; Drewes, Jochen

    2016-10-22

    HIV testing and serostatus awareness are essential to implement biomedical strategies (treatment as prevention; oral chemoprophylaxis), and for effective serostatus-based behaviours (HIV serosorting; strategic positioning). The analysis focuses on the associations between reported sexual risks, the perceived risk for HIV infection, and HIV testing behaviour in order to identify the most relevant barriers for HIV test uptake among MSM living in Germany. MSM were recruited to a nationwide anonymous online-survey in 2013 on MSM social networking/dating sites. Questions covered testing behaviours, reasons for testing decisions, and HIV risk perception (5-point scale). Additional questions addressed arguments in favour of home/ home collection testing (HT). Using descriptive statistics and logistic regression we compared men reporting recent HIV testing (RT; previous 12 month) with men never tested (NT) in a subsample not previously diagnosed with HIV and reporting ≥2 episodes of condomless anal intercourse (CLAI) with a non-steady partner of unknown HIV serostatus in the previous 12 months. The subsample consisted of 775 RT (13 % of RT) and 396 NT (7 % of NT). The number of CLAI episodes in the last 12 months with non-steady partners of unknown HIV status did not differ significantly between the groups, but RT reported significantly higher numbers of partners (>5 AI partners: 65 vs. 44 %). While perceived risks regarding last AI were comparable between the groups, 49vs. 30 % NT were risks (67 %) and routine testing (49 %) were the most common testing reasons for RT, while the strong belief not to be infected (59 %) and various worries (41 %) and fears of testing positive (35 %) were predominant reasons of NT. Greater anonymity (aOR 3.2; 2.4-4.4), less embarrassment, (aOR 2.8; 1.9-4.1), and avoiding discussions on sexual behaviour (aOR 1.6; 1.1-2.2) were emphasized in favour of HT by NT. Perceived partner knowledge and reasons reflecting perceived gay- and

  4. Successful adalimumab treatment of a psoriasis vulgaris patient with hemodialysis for renal failure: A case report and a review of the previous reports on biologic treatments for psoriasis patients with hemodialysis for renal failure.

    Science.gov (United States)

    Kusakari, Yoshiyuki; Yamasaki, Kenshi; Takahashi, Toshiya; Tsuchiyama, Kenichiro; Shimada-Omori, Ryoko; Nasu-Tamabuchi, Mei; Aiba, Setsuya

    2015-07-01

    The efficacy and safety of biologic treatments have been established in patients with moderate to severe psoriasis, but there are few reports on biologic therapy for patients with psoriasis complicated by end-stage renal failure on hemodialysis (HD). In this report, we demonstrated the efficacy and safety of adalimumab for patients with severe psoriasis on HD. A 46-year-old Japanese man with a 14-year history of psoriasis was referred to our clinic in September 2009. He had developed hypertension and renal failure during a 7-year history of cyclosporin treatment. With the infliximab treatment, he achieved 75% improvement of the Psoriasis Area and Severity Index (PASI) score within 3 months from the PASI of 42.3 before the treatment. However, his renal failure gradually deteriorated, and HD was initiated at 1 year after the introduction of infliximab. Because of hydration during the i.v. injection of infliximab, he developed pulmonary edema with every infliximab treatment after starting HD. We switched to ustekinumab treatment, but his psoriasis was not improved. Then, we switched to adalimumab and achieved a PASI-100 response within 2 months. The patient received adalimumab treatment for more than a year without any adverse effects. In addition to our case, five articles reported cases of psoriasis patients with renal failure on HD who were treated with biologics. The psoriatic lesions were improved by biologics in these cases, and no severe adverse effects on the renal function were reported. Thus, biologics are a reasonable treatment option for patients with severe psoriasis with renal failure on HD. © 2015 Japanese Dermatological Association.

  5. A Simple and Effective Isocratic HPLC Method for Fast Identification and Quantification of Surfactin

    International Nuclear Information System (INIS)

    Muhammad Qadri Effendy Mubarak; Abdul Rahman Hassan; Aidil Abdul Hamid; Sahaid Khalil; Mohd Hafez Mohd Isa

    2015-01-01

    The aim of this study was to establish a simple, accurate and reproducible method for the identification and quantification of surfactin using high-performance liquid chromatography (HPLC). Previously reported method of identification and quantification of surfactin were time consuming and requires a large quantity of mobile phase. The new method was achieved by application of Chromolith® high performance RP-18 (100 x 4.6 mm, 5 μm) as the stationary phase and optimization of mobile phase ratio and flow rate. Mobile phase consisted of acetonitrile (ACN) and 3.8 mM trifluroacetic acid (TFA) solution of 80:20 ratio at flow rate of 2.2 mL/ min was obtained as the optimal conditions. Total elution time of the obtained surfactin peaks was four times quicker than various methods previously reported in the literature. The method described here allowed for fine separation of surfactin in standard sample (98 % purity) and surfactin in fermentation broth. (author)

  6. Quantification of furanoheliangolides by HPLC and GC Quantificação dos furanoeliangolidos por HPLC e CG

    Directory of Open Access Journals (Sweden)

    Pierre Alexandre dos Santos

    2003-09-01

    Full Text Available The development and comparison of two analytical methods (HPLC and GC for the quantification of the most common furanoheliangolides from Lychnophora is reported in this paper. Both methods are sensitive and suitable for quantification of these metabolites.Neste trabalho são descritos o desenvolvimento e comparação de dois métodos analíticos (CLAE e CG para quantificação dos furanoeliangolidos mais comuns em Lychnophora.Ambos os métodos são sensíveis e adequados para a quantificação desses metabólitos.

  7. Quantification of furanoheliangolides by HPLC and GC Quantificação dos furanoeliangolidos por HPLC e CG

    OpenAIRE

    Pierre Alexandre dos Santos; Izabel Cristina Casanova Turati; José Carlos Tomaz; Norberto Peporine Lopes

    2003-01-01

    The development and comparison of two analytical methods (HPLC and GC) for the quantification of the most common furanoheliangolides from Lychnophora is reported in this paper. Both methods are sensitive and suitable for quantification of these metabolites.Neste trabalho são descritos o desenvolvimento e comparação de dois métodos analíticos (CLAE e CG) para quantificação dos furanoeliangolidos mais comuns em Lychnophora.Ambos os métodos são sensíveis e adequados para a quantificação desses m...

  8. Re-purification of labelled ferritin antigen with HPLC

    International Nuclear Information System (INIS)

    Zhang Haoyi; Jin Lichun

    2002-01-01

    Objective: To improve the quality of long-term stored labelled ferritin antigen with HPLC. Methods: The antigen was analyzed and purified with HPLC and again analyzed with RIA afterwards. Results: Ferritin antigen underwent significant polymerization after long-term (aggregation) storage. After re-purification with HPLC, its immuno-activity and labelled specific radioactivity were both significantly improved. Conclusion: Quality of stored ferritin RIA kit could be greatly improved after re-purification with HPLC

  9. Environmentally evaluated HPLC-ELSD method to monitor enzymatic synthesis of a non-ionic surfactant.

    Science.gov (United States)

    Gaber, Yasser; Akerman, Cecilia Orellana; Hatti-Kaul, Rajni

    2014-01-01

    N-Lauroyl-N-methylglucamide is a biodegradable surfactant derived from renewable resources. In an earlier study, we presented an enzymatic solvent-free method for synthesis of this compound. In the present report, the HPLC method developed to follow the reaction between lauric acid/methyl laurate and N-methyl glucamine (MEG) and its environmental assessment are described. Use of ultraviolet (UV) absorption or refractive index (RI) detectors did not allow the detection of N-methyl glucamine (MEG). With Evaporative light scattering detector ELSD, it was possible to apply a gradient elution, and detect MEG with a limit of detection, LOD = 0.12 μg. A good separation of the peaks: MEG, lauric acid, product (amide) and by-product (amide-ester) was achieved with the gradient program with a run time of 40 min. The setting of ELSD detector was optimized using methyl laurate as the analyte. LC-MS/MS was used to confirm the amide and amide-ester peaks. We evaluated the greenness of the developed method using the freely available software HPLC-Environmental Assessment Tool (HPLC-EAT) and the method got a scoring of 73 HPLC-EAT units, implying that the analytical procedure was more environmentally benign compared to some other methods reported in literature whose HPLC-EAT values scored up to 182. Use of ELSD detector allowed the detection and quantification of the substrates and the reaction products of enzymatic synthesis of the surfactant, N-lauroyl-N-methylglucamide. The developed HPLC method has acceptable environmental profile based on HPLC-EAT evaluation.

  10. Improved method for HPLC analysis of polyamines, agmatine and aromatic monoamines in plant tissue

    Science.gov (United States)

    Slocum, R. D.; Flores, H. E.; Galston, A. W.; Weinstein, L. H.

    1989-01-01

    The high performance liquid chromatographic (HPLC) method of Flores and Galston (1982 Plant Physiol 69: 701) for the separation and quantitation of benzoylated polyamines in plant tissues has been widely adopted by other workers. However, due to previously unrecognized problems associated with the derivatization of agmatine, this important intermediate in plant polyamine metabolism cannot be quantitated using this method. Also, two polyamines, putrescine and diaminopropane, also are not well resolved using this method. A simple modification of the original HPLC procedure greatly improves the separation and quantitation of these amines, and further allows the simulation analysis of phenethylamine and tyramine, which are major monoamine constituents of tobacco and other plant tissues. We have used this modified HPLC method to characterize amine titers in suspension cultured carrot (Daucas carota L.) cells and tobacco (Nicotiana tabacum L.) leaf tissues.

  11. HIV risk perception and testing behaviours among men having sex with men (MSM reporting potential transmission risks in the previous 12 months from a large online sample of MSM living in Germany

    Directory of Open Access Journals (Sweden)

    Ulrich Marcus

    2016-10-01

    Full Text Available Abstract Background HIV testing and serostatus awareness are essential to implement biomedical strategies (treatment as prevention; oral chemoprophylaxis, and for effective serostatus-based behaviours (HIV serosorting; strategic positioning. The analysis focuses on the associations between reported sexual risks, the perceived risk for HIV infection, and HIV testing behaviour in order to identify the most relevant barriers for HIV test uptake among MSM living in Germany. Methods MSM were recruited to a nationwide anonymous online-survey in 2013 on MSM social networking/dating sites. Questions covered testing behaviours, reasons for testing decisions, and HIV risk perception (5-point scale. Additional questions addressed arguments in favour of home/ home collection testing (HT. Using descriptive statistics and logistic regression we compared men reporting recent HIV testing (RT; previous 12 month with men never tested (NT in a subsample not previously diagnosed with HIV and reporting ≥2 episodes of condomless anal intercourse (CLAI with a non-steady partner of unknown HIV serostatus in the previous 12 months. Results The subsample consisted of 775 RT (13 % of RT and 396 NT (7 % of NT. The number of CLAI episodes in the last 12 months with non-steady partners of unknown HIV status did not differ significantly between the groups, but RT reported significantly higher numbers of partners (>5 AI partners: 65 vs. 44 %. While perceived risks regarding last AI were comparable between the groups, 49vs. 30 % NT were <30 years, lived more often in towns/villages <100,000 residents (60 vs. 39 %, were less out-particularly towards care providers-about being attracted to men (aOR 10.1; 6.9–14.8, more often identified as bisexual (aOR 3.5; 2.5–4.8, and reported lower testing intentions (aOR 0.08; 0.06–0.11. Perceived risks (67 % and routine testing (49 % were the most common testing reasons for RT, while the strong belief not to be infected

  12. Retinol analysis in dried blood spots by HPLC.

    Science.gov (United States)

    Craft, N E; Haitema, T; Brindle, L K; Yamini, S; Humphrey, J H; West, K P

    2000-04-01

    There are many advantages to measuring vitamin A in dried blood spots (DBS) from a finger prick as compared to plasma collected by venipuncture. The advantages include easier collection, transport and storage; accessibility to younger and more remote populations; and decreased risk of disease transmission. We describe a method for the extraction of retinol from DBS for analysis by HPLC and initial comparison to plasma retinol. The effects of various buffers, detergents, antioxidants and chelators were evaluated to establish the most effective approach to elute the retinol: retinol binding protein (holo-RBP) complex from the blood collection cards. The process involves ultrasonic agitation to elute holo-RBP into a phosphate buffer containing an antioxidant and metal chelator. The holo-RBP complex was denatured by the addition of ethanol containing additional antioxidants permitting the extraction of free retinol into hexane. Following solvent evaporation, the extract was dissolved in methanol for HPLC analysis. The initial measured retinol levels in freshly collected DBS declined for 6-10 d whether stored at 25, 4 or -20 degrees C, but remained consistent thereafter (homeostatic). By incorporating a "recovery/volume adjustment" factor, measured retinol values in homeostatic DBS were adjusted to the equivalent of plasma retinol. For 17 normal adults, the correlation coefficient was 0.90 between plasma retinol and adjusted DBS retinol in samples that had been stored at -70 degrees C for < 9 mo. The use of this new sample matrix for vitamin A assessment will allow access to previously unavailable populations.

  13. HPLC assisted Raman spectroscopic studies on bladder cancer

    Science.gov (United States)

    Zha, W. L.; Cheng, Y.; Yu, W.; Zhang, X. B.; Shen, A. G.; Hu, J. M.

    2015-04-01

    We applied confocal Raman spectroscopy to investigate 12 normal bladder tissues and 30 tumor tissues, and then depicted the spectral differences between the normal and the tumor tissues and the potential canceration mechanism with the aid of the high-performance liquid chromatographic (HPLC) technique. Normal tissues were demonstrated to contain higher tryptophan, cholesterol and lipid content, while bladder tumor tissues were rich in nucleic acids, collagen and carotenoids. In particular, β-carotene, one of the major types of carotenoids, was found through HPLC analysis of the extract of bladder tissues. The statistical software SPSS was applied to classify the spectra of the two types of tissues according to their differences. The sensitivity and specificity of 96.7 and 66.7% were obtained, respectively. In addition, different layers of the bladder wall including mucosa (lumps), muscle and adipose bladder tissue were analyzed by Raman mapping technique in response to previous Raman studies of bladder tissues. All of these will play an important role as a directive tool for the future diagnosis of bladder cancer in vivo.

  14. Measurement of menadione in urine by HPLC.

    Science.gov (United States)

    Al Rajabi, Ala; Peterson, James; Choi, Sang-Woon; Suttie, John; Barakat, Susan; Booth, Sarah L

    2010-09-15

    Menadione is a metabolite of vitamin K that is excreted in urine. A high performance liquid chromatography (HPLC) method using a C(30) column, post-column zinc reduction and fluorescence detection was developed to measure urinary menadione. The mobile phase was composed of 95% methanol with 0.55% aqueous solution and 5% DI H(2)O. Menaquinone-2 (MK-2) was used as an internal standard. The standard calibration curve was linear with a correlation coefficient (R(2)) of 0.999 for both menadione and MK-2. The lower limit of quantification (LLOQ) was 0.3pmole menadione/mL urine. Sample preparation involved hydrolysis of menadiol conjugates and oxidizing the released menadiol to menadione. Using this method, urinary menadione was shown to increase in response to 3 years of phylloquinone supplementation. This HPLC method is a sensitive and reproducible way to detect menadione in urine. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  15. Detection and quantification of new psychoactive substances (NPSs) within the evolved "legal high" product, NRG-2, using high performance liquid chromatography-amperometric detection (HPLC-AD).

    Science.gov (United States)

    Zuway, Khaled Y; Smith, Jamie P; Foster, Christopher W; Kapur, Nikil; Banks, Craig E; Sutcliffe, Oliver B

    2015-09-21

    The global increase in the production and abuse of cathinone-derived New Psychoactive Substances (NPSs) has developed the requirement for rapid, selective and sensitive protocols for their separation and detection. Electrochemical sensing of these compounds has been demonstrated to be an effective method for the in-field detection of these substances, either in their pure form or in the presence of common adulterants, however, the technique is limited in its ability to discriminate between structurally related cathinone-derivatives (for example: (±)-4′-methylmethcathinone (4-MMC, 2a) and (±)-4′-methyl-N-ethylmethcathinone (4-MEC, 2b) when they are both present in a mixture. In this paper we demonstrate, for the first time, the combination of HPLC-UV with amperometric detection (HPLC-AD) for the qualitative and quantitative analysis of 4-MMC and 4-MEC using either a commercially available impinging jet (LC-FC-A) or custom-made iCell channel (LC-FC-B) flow-cell system incorporating embedded graphite screen-printed macroelectrodes. The protocol offers a cost-effective, reproducible and reliable sensor platform for the simultaneous HPLC-UV and amperometric detection of the target analytes. The two systems have similar limits of detection, in terms of amperometric detection [LC-FC-A: 14.66 μg mL(-1) (2a) and 9.35 μg mL(-1) (2b); LC-FC-B: 57.92 μg mL(-1) (2a) and 26.91 μg mL(-1) (2b)], to the previously reported oxidative electrochemical protocol [39.8 μg mL(-1) (2a) and 84.2 μg mL(-1) (2b)], for two synthetic cathinones, prevalent on the recreational drugs market. Though not as sensitive as standard HPLC-UV detection, both flow cells show a good agreement, between the quantitative electroanalytical data, thereby making them suitable for the detection and quantification of 4-MMC and 4-MEC, either in their pure form or within complex mixtures. Additionally, the simultaneous HPLC-UV and amperometric detection protocol detailed herein shows a marked improvement

  16. [Spectrophotometric and HPLC evaluation of ceftazidime stability].

    Science.gov (United States)

    Palade, B; Cioroiu, B; Lazăr, Doina; Corciovă, Andreia; Lazăr, M I

    2010-01-01

    In this paper we followed up the stability of ceftazidime, raw material used in drug industry. Matherials and methods: We used three spectrophotometric methods based on ceftazidime property to form complexes with p-chloranilic acid (ac. p-CA), 3-methylbenzothiazolin-2-on hydrazone (MBTH) and N-(1-naphtil) etilendiamine (NEDA) and a chromatographic method (HPLC). Our results revealed that the substances analyzed maintained minimum content allowable.

  17. Validation of previously reported predictors for radiation-induced hypothyroidism in nasopharyngeal cancer patients treated with intensity-modulated radiation therapy, a post hoc analysis from a Phase III randomized trial.

    Science.gov (United States)

    Lertbutsayanukul, Chawalit; Kitpanit, Sarin; Prayongrat, Anussara; Kannarunimit, Danita; Netsawang, Buntipa; Chakkabat, Chakkapong

    2018-05-10

    This study aimed to validate previously reported dosimetric parameters, including thyroid volume, mean dose, and percentage thyroid volume, receiving at least 40, 45 and 50 Gy (V40, V45 and V50), absolute thyroid volume spared (VS) from 45, 50 and 60 Gy (VS45, VS50 and VS60), and clinical factors affecting the development of radiation-induced hypothyroidism (RHT). A post hoc analysis was performed in 178 euthyroid nasopharyngeal cancer (NPC) patients from a Phase III study comparing sequential versus simultaneous-integrated boost intensity-modulated radiation therapy. RHT was determined by increased thyroid-stimulating hormone (TSH) with or without reduced free thyroxin, regardless of symptoms. The median follow-up time was 42.5 months. The 1-, 2- and 3-year freedom from RHT rates were 78.4%, 56.4% and 43.4%, respectively. The median latency period was 21 months. The thyroid gland received a median mean dose of 53.5 Gy. Female gender, smaller thyroid volume, higher pretreatment TSH level (≥1.55 μU/ml) and VS60 treatment planning.

  18. Quality control of radiopharmaceuticals with HPLC using aqueous size exclusion spherogel column

    International Nuclear Information System (INIS)

    Vallabhajosula, S.; Goldsmith, S.J.; Lipszyc, H.

    1982-01-01

    The application of HPLC for the analysis and quality control of 99 Tc-radiopharmaceuticals, using a weakly basic anion exchange column, has been reported. This HPLC method for the separation of the components is based on molecular size. 99 Tc-MDP, 99 Tc-HDP and 99 Tc-DTPA were analysed and UV absorption studies carried out on the components. Components of the 99 Tc-MDP separation were injected into rabbits and renal excretion and serial images studied. (U.K.)

  19. Previously unknown species of Aspergillus.

    Science.gov (United States)

    Gautier, M; Normand, A-C; Ranque, S

    2016-08-01

    The use of multi-locus DNA sequence analysis has led to the description of previously unknown 'cryptic' Aspergillus species, whereas classical morphology-based identification of Aspergillus remains limited to the section or species-complex level. The current literature highlights two main features concerning these 'cryptic' Aspergillus species. First, the prevalence of such species in clinical samples is relatively high compared with emergent filamentous fungal taxa such as Mucorales, Scedosporium or Fusarium. Second, it is clearly important to identify these species in the clinical laboratory because of the high frequency of antifungal drug-resistant isolates of such Aspergillus species. Matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF MS) has recently been shown to enable the identification of filamentous fungi with an accuracy similar to that of DNA sequence-based methods. As MALDI-TOF MS is well suited to the routine clinical laboratory workflow, it facilitates the identification of these 'cryptic' Aspergillus species at the routine mycology bench. The rapid establishment of enhanced filamentous fungi identification facilities will lead to a better understanding of the epidemiology and clinical importance of these emerging Aspergillus species. Based on routine MALDI-TOF MS-based identification results, we provide original insights into the key interpretation issues of a positive Aspergillus culture from a clinical sample. Which ubiquitous species that are frequently isolated from air samples are rarely involved in human invasive disease? Can both the species and the type of biological sample indicate Aspergillus carriage, colonization or infection in a patient? Highly accurate routine filamentous fungi identification is central to enhance the understanding of these previously unknown Aspergillus species, with a vital impact on further improved patient care. Copyright © 2016 European Society of Clinical Microbiology and

  20. Uncertainty budget for final assay of a pharmaceutical product based on RP-HPLC

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Anglov, Thomas; Byrialsen, Kirsten

    2003-01-01

    ). The reported example illustrates the estimation of uncertainty for the final determination of a protein concentration by HPLC using UV detection, using the approach described by EURACHEM/CITAC. The combined standard uncertainty for a protein concentration of 2400 mumol/L was estimated to be 14 mumol/L. All...

  1. Ionisation constants of radiopharmaceuticals by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Stylli, C.G.; Theobald, A.E.

    It has long been recognised that the pKsub(a) of drugs and radiopharmaceuticals is an important determinant of their biological distribution. In this study an HPLC method for pKa measurement has been developed for radiotracers. It has been validated with several amines and used to estimate the pKsub(a) values of some Tc-99m PnAO complexes by observing the change in chromatographic retention with change in mobile phase pH. The pKsub(a) values were estimated from the data by three methods: derivative analysis, quadratic regression, and the Henderson - Hasselbalch equation.

  2. Ionisation constants of radiopharmaceuticals by HPLC

    International Nuclear Information System (INIS)

    Stylli, C.G.; Theobald, A.E.

    1986-01-01

    It has long been recognised that the pKsub(a) of drugs and radiopharmaceuticals is an important determinant of their biological distribution. In this study an HPLC method for pKa measurement has been developed for radiotracers. It has been validated with several amines and used to estimate the pKsub(a) values of some Tc-99m PnAO complexes by observing the change in chromatographic retention with change in mobile phase pH. The pKsub(a) values were estimated from the data by three methods: derivative analysis, quadratic regression, and the Henderson - Hasselbalch equation. (author)

  3. HPLC determination of caffeine in coffee beverage

    Science.gov (United States)

    Fajara, B. E. P.; Susanti, H.

    2017-11-01

    Coffee is the second largest beverage which is consumed by people in the world, besides the water. One of the compounds which contained in coffee is caffeine. Caffeine has the pharmacological effect such as stimulating the central nervous system. The purpose of this study is to determine the level of caffeine in coffee beverages with HPLC method. Three branded coffee beverages which include in 3 of Top Brand Index 2016 Phase 2 were used as samples. Qualitative analysis was performed by Parry method, Dragendorff reagent, and comparing the retention time between sample and caffeine standard. Quantitative analysis was done by HPLC method with methanol-water (95:5v/v) as mobile phase and ODS as stationary phasewith flow rate 1 mL/min and UV 272 nm as the detector. The level of caffeine data was statistically analyzed using Anova at 95% confidence level. The Qualitative analysis showed that the three samples contained caffeine. The average of caffeine level in coffee bottles of X, Y, and Z were 138.048 mg/bottle, 109.699 mg/bottle, and 147.669 mg/bottle, respectively. The caffeine content of the three coffee beverage samples are statistically different (pcoffee beverage samples were not meet the requirements set by the Indonesian Standard Agency of 50 mg/serving.

  4. Radio-activity detectors in HPLC

    International Nuclear Information System (INIS)

    Kremers, H.D.

    1984-01-01

    Two different approaches were adopted to put the eluate from the HPLC into contact with the scintillator, i.e. a homogeneous and a heterogeneous system. In the heterogeneous system, the eluate runs directly through a cell filled with a fine-grain solid scintillator. In the homogeneous system, a liquid scintillator is admixed to the eluate or to a proportion of the eluate before flowing through the measurement cell. Both systems are contrasted with the fractionation method according to the criterias of handling, rapidity of analysis and facility cost. On-line detection of radio-activity will be easily settled for when comparing its investment cost with those of materials consumed in fractionation. A device prepared for scintillator admixture contains an integrated scintillator pump and a mixer but is suitable for application of solid scintillator cells, too. Such a system features a wider range of practical applications than a device exclusively designed for the heterogeneous system. A further asset of the detectors in the fact that they are adapted in their performance to up-to-date HPLC facilities in terms of speed and resolution. (orig./HP) [de

  5. Ellagitannin composition of blackberry as determined by HPLC-ESI-MS and MALDI-TOF-MS.

    Science.gov (United States)

    Hager, Tiffany J; Howard, Luke R; Liyanage, Rohana; Lay, Jackson O; Prior, Ronald L

    2008-02-13

    Blackberries ( Rubus sp.) were evaluated by high-performance liquid chromatography-electrospray ionization-mass spectrometry (HPLC-ESI-MS) and matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry (MALDI-TOF-MS) to identify the ellagitannins present in flesh, torus (receptacle tissue), and seeds. Most ellagitannins were present (or detectable) only in seed tissues. Ellagitannins identified by HPLC-ESI-MS in the seeds included pedunculagin, casuarictin/potentillin, castalagin/vescalagin, lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D. For several of the ellagitannins, isomeric separation was also obtained. The MALDI-TOF-MS analysis was primarily utilized to evaluate and identify high molecular mass (>1000 Da) ellagitannins. The MALDI analysis verified the presence of the ellagitannins identified by HPLC-ESI-MS including lambertianin A/sanguiin H-6, lambertianin C, and lambertianin D, but the analysis also indicated the presence of several other compounds that were most likely ellagitannins based on the patterns observed in the masses (i.e., loss or addition of a gallic acid moiety to a known ellagitannin). This study determined the presence of several possible isomeric forms of ellagitannins previously unidentified in fruit and presents a possible analytical HPLC method for the analysis of the major ellagitannins present in the fruit.

  6. Recent developments in HPLC analysis of β-blockers in biological samples.

    Science.gov (United States)

    Saleem, Kishwar; Ali, Imran; Kulsum, Umma; Aboul-Enein, Hassan Y

    2013-09-01

    β-Adrenergic blockers represent a very important class of drugs that are used worldwide for treating various cardiac diseases. The present article describes the state-of-the art of analyses of β-adrenergic blockers using high-performance liquid chromatography (HPLC). Sample preparation techniques such as liquid-liquid extraction, solid-phase extraction and solid-phase microextraction have been discussed, which are essential prior to HPLC analysis. Additionally, applications of liquid chromatography coupled with tandem mass spectrometry are included. HPLC methods have been reported to include 0.6-26 min as the run times and 0.01 ng/mL to 25 µg/mL as detection limits. The most commonly used columns were C18 with various buffers as the mobile phases, along with various organic modifiers. The optimization of HPLC conditions has been discussed. It has been observed that the reported methods are quite satisfactory for the analyses of β-adrenergic blockers in biological samples. Future perspectives in the hyphenation of solid-phase microextraction-nano-liquid chromatography-tandem mass spectrometry have also been highlighted to achieve detections at nanogram and picogram levels. The present article is very useful for academicians, scientists, drug and pharmaceutical personnel and government regulatory authorities.

  7. Reversed Phase Column HPLC-ICP-MS Conditions for Arsenic Speciation Analysis of Rice Flour.

    Science.gov (United States)

    Narukawa, Tomohiro; Matsumoto, Eri; Nishimura, Tsutomu; Hioki, Akiharu

    2015-01-01

    New measurement conditions for arsenic speciation analysis of rice flour were developed using HPLC-ICP-MS equipped with a reversed phase ODS column. Eight arsenic species, namely, arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide (TMAO), tetramethylarsonium (TeMA), arsenobetaine (AsB) and arsenocholine (AsC), were separated and determined under the proposed conditions. In particular, As(III) and MMAA and DMAA and AsB were completely separated using a newly proposed eluent containing ammonium dihydrogen phosphate. Importantly, the sensitivity changes, in particular those of As(V) and As(III) caused by coexisting elements and by complex matrix composition, which had been problematical in previously reported methods, were eliminated. The new eluent can be applied to C8, C18 and C30 ODS columns with the same effectiveness and with excellent repeatability. The proposed analytical method was successfully applied to extracts of rice flour certified reference materials.

  8. Capillary-HPLC with tandem mass spectrometry in analysis of alkaloid dyestuffs - a new approach.

    Science.gov (United States)

    Dąbrowski, Damian; Lech, Katarzyna; Jarosz, Maciej

    2018-05-01

    Development of the identification method of alkaloid compounds in Amur cork tree as well as not examined so far Oregon grape and European Barberry shrubs are presented. The novel approach to separation of alkaloids was applied and the capillary-high-performance liquid chromatography (capillary-HPLC) system was used, which has never previously been reported for alkaloid-based dyestuffs analysis. Its optimization was conducted with three different stationary phases (unmodified octadecylsilane-bonded silica, octadecylsilane modified with polar groups and silica-bonded pentaflourophenyls) as well as with different solvent buffers. Detection of the isolated compounds was carried out using diode-array detector (DAD) and tandem mass spectrometer with electrospray ionization (ESI MS/MS). The working parameters of ESI were optimized, whereas the multiple reactions monitoring (MRM) parameters of MS/MS detection were chosen based on the product ion spectra of the quasi-molecular ions. Calibration curve of berberine has been estimated (y = 1712091x + 4785.03 with the correlation coefficient 0.9999). Limit of detection and limit of quantification were calculated to be 3.2 and 9.7 ng/mL, respectively. Numerous alkaloids (i.e., berberine, jatrorrhizine and magnoflorine, as well as phellodendrine, menisperine and berbamine) were identified in the extracts from alkaloid plants and silk and wool fibers dyed with these dyestuffs, among them their markers. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Electrochemical Detectors in HPLC and Ion Chromatography.

    Science.gov (United States)

    Horvai, George; Pungor, ErnÕ

    1989-01-01

    Back in 1952, the renowned Polish electrochemist Wiktor Kemula introduced chromato-polarography, 1 i.e., polaro-graphic detection for liquid chromatography. This technique continued to develop slowly until the early 1970s (for a review see Reference 2) when modem high-performance liquid chromatography (HPLC) emerged. This new, highly efficient chromatographc method could only be. used with detectors ensuring low dispersion. It was not easy to modify the dropping mercury electrode cells to satisfy this requirement. However, at the same time, electroanalytical chemists, who already had much experience in using carbon-based electrodes for oxidative detection in flow analysis, put forward the idea of oxidative amperometric detection in liquid chromatography. 3,4 In this technique, solid or quasi-solid (paste) electrodes were used and this made possible the construction of miniaturized cells with just a few microliter volume.

  10. Analysis of xanthophylls in corn by HPLC.

    Science.gov (United States)

    Moros, E E; Darnoko, D; Cheryan, M; Perkins, E G; Jerrell, J

    2002-10-09

    An HPLC method was developed using the C-30 carotenoid column to separate and identify the major xanthophylls in corn (lutein, zeaxanthin, and beta-cryptoxanthin). A photodiode array detector and a mobile phase consisting of methyl tert-butyl ether/methanol/water was used. All three xanthophylls eluted in less than 25 min. Yellow dent corn had a total xanthophyll content of 21.97 microg/g with lutein content of 15.7 microg/g, zeaxanthin content of 5.7 microg/g, and beta-cryptoxanthin of 0.57 microg/g. Commercial corn gluten meal had a 7 times higher concentration of xanthophylls (145 microg/g), and deoiled corn contained 18 microg/g, indicating that the xanthophylls are probably bound to the zein fraction of corn proteins.

  11. Optimizing Chromatographic Separation: An Experiment Using an HPLC Simulator

    Science.gov (United States)

    Shalliker, R. A.; Kayillo, S.; Dennis, G. R.

    2008-01-01

    Optimization of a chromatographic separation within the time constraints of a laboratory session is practically impossible. However, by employing a HPLC simulator, experiments can be designed that allow students to develop an appreciation of the complexities involved in optimization procedures. In the present exercise, a HPLC simulator from "JCE…

  12. HPLC-ESR techniques for detection of complex trapped radicals

    International Nuclear Information System (INIS)

    Tu Tiecheng; Dong Jirong; Lin Nianyun; Xie Leidong; Liu Rengzhong

    1992-01-01

    High performance liquid chromatography (HPLC) and ESR combined examination of radical species is an advanced techniques for separation and identification of complex radical species. At SRCL, Waters 990 HPLC has been used to separate the complex trapped radicals and Varian E-112 ESR spectrometer to record the spectra of single trapped radicals after HPLC separation. The advantages of the combined techniques are described as bellow: HPLC is used to separate the long-lived complex trapped radicals derived from reaction of short-lived radicals with spin trap. ESR spectra from single trapped radicals, obtained following HPLC separation of complex trapped radicals, are recorded one by one and well resolved. The structures of short-lived radicals can be inferred from the ESR spectra of the long-lived trapped radicals

  13. Subsequent childbirth after a previous traumatic birth.

    Science.gov (United States)

    Beck, Cheryl Tatano; Watson, Sue

    2010-01-01

    Nine percent of new mothers in the United States who participated in the Listening to Mothers II Postpartum Survey screened positive for meeting the Diagnostic and Statistical Manual of Mental Disorders, Fourth Edition criteria for posttraumatic stress disorder after childbirth. Women who have had a traumatic birth experience report fewer subsequent children and a longer length of time before their second baby. Childbirth-related posttraumatic stress disorder impacts couples' physical relationship, communication, conflict, emotions, and bonding with their children. The purpose of this study was to describe the meaning of women's experiences of a subsequent childbirth after a previous traumatic birth. Phenomenology was the research design used. An international sample of 35 women participated in this Internet study. Women were asked, "Please describe in as much detail as you can remember your subsequent pregnancy, labor, and delivery following your previous traumatic birth." Colaizzi's phenomenological data analysis approach was used to analyze the stories of the 35 women. Data analysis yielded four themes: (a) riding the turbulent wave of panic during pregnancy; (b) strategizing: attempts to reclaim their body and complete the journey to motherhood; (c) bringing reverence to the birthing process and empowering women; and (d) still elusive: the longed-for healing birth experience. Subsequent childbirth after a previous birth trauma has the potential to either heal or retraumatize women. During pregnancy, women need permission and encouragement to grieve their prior traumatic births to help remove the burden of their invisible pain.

  14. [Development of Tianma HPLC fingerprint and discriminant analysis].

    Science.gov (United States)

    Xiao, Jia-Jia; Huang, Hong; Lei, You-Cheng; Lin, Ting-Wen; Ma, Yue; Zhang, Jing; Zhang, Xing-Guo; Zhang, Da-Quan; Lv, Guang-Hua

    2017-07-01

    Tianma(the tuber of Gastrodia eleta) is a widely used and pricy Chinese herb. Its counterfeits are often found in herbal markets, which are the plant materials with similar macroscopic characteristics of Tianma. Moreover, the prices of Winter Tianma(cultivated Tianma) and Spring Tianma(mostly wild Tianma) have significant difference. However, it is difficult to identify the true or false, good or bad quality of Tianma samples. Thus, a total of 48 Tianma samples with different characteristics(including Winter Tianma, Spring Tianma, slice, powder, etc.) and 9 plant species 10 samples of Tianma counterfeits were collected and analyzed by HPLC-DAD-MS techniques. After optimizing the procedure of sample preparation, chromatographic and mass-spectral conditions, the HPLC chromatograms of all those samples were collected and compared. The similarities and Fisher discriminant analysis were further conducted between the HPLC chromatograms of Tianma and counterfeit, Winter Tianma and Spring Tianma. The results showed the HPLC chromatograms of 48 Tianma samples were similar at the correlation coefficient more than 0.848(n=48). Their mean chromatogram was simulated and used as Tianma HPLC fingerprint. There were 11 common peaks on the HPLC chromatograms of Tianma, in which 6 main peaks were chosen as characteristic peaks and identified as gastrodin, p-hydroxybenzyl alcohol, parishin A, parishin B, parishin C, parishin E, respectively by comparison of the retention time, UV and MS data with those of standard chemical compounds. All the six chemical compounds are bioactive in Tianma. However, the HPLC chromatograms of the 10 counterfeit samples were significantly different from Tianma fingerprint. The correlation coefficients between HPLC fingerprints of Tianma with the HPLC chromatograms of counterfeits were less than 0.042 and the characteristic peaks were not observed on the HPLC chromatograms of these counterfeit samples. It indicated the true or false Tianma can be

  15. Direct 13C NMR Detection in HPLC Hyphenation Mode

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils

    2012-01-01

    Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments...... application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings...

  16. DETERMINATION AND VALIDATION OF MEBHYDROLINE NAPADISYLATE IN TABLETS BY HPLC

    Directory of Open Access Journals (Sweden)

    Lestyo Wulandari

    2010-06-01

    Full Text Available An accurate and sensitive HPLC method has been developed for the determination of mebhydroline napadisylate in the tablet. The Chromatography was performed on a reversed phase C-18 column, using a mobile phase of acetonitrile : ammonia 25% (80 : 20 v/v at ambient temperature 25±5 °C and UV detection operates at 320 nm in an overall analysis time of about 15 min, based on peak area. This HPLC method is selective, precise, and accurate and can be used for routine analysis of pharmaceutical preparation in industrial quality-control laboratories.   Keywords : HPLC, mebhydroline napadisylate, validation

  17. Determination of carbonyl compounds in air by HPLC; Determinacion de compuestos carbonilicos en aire por HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, S; Perez, R M; Campos, A; Gonzalez, D

    1995-07-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs.

  18. Identification and Quantitation of Asparagine and Citrulline Using High-Performance Liquid Chromatography (HPLC)

    OpenAIRE

    Bai, Cheng; Reilly, Charles C.; Wood, Bruce W.

    2007-01-01

    High-performance liquid chromatography (HPLC) analysis was used for identification of two problematic ureides, asparagine and citrulline. We report here a technique that takes advantage of the predictable delay in retention time of the co-asparagine/citrulline peak to enable both qualitative and quantitative analysis of asparagine and citrulline using the Platinum EPS reverse-phase C18 column (Alltech Associates). Asparagine alone is eluted earlier than citrulline alone, but when both of them...

  19. Automated Liquid Microjunction Surface Sampling-HPLC-MS/MS Analysis of Drugs and Metabolites in Whole-Body Thin Tissue Sections

    Energy Technology Data Exchange (ETDEWEB)

    Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2013-01-01

    A fully automated liquid extraction-based surface sampling system utilizing a commercially available autosampler coupled to high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) detection is reported. Discrete spots selected for droplet-based sampling and automated sample queue generation for both the autosampler and MS were enabled by using in-house developed software. In addition, co-registration of spatially resolved sampling position and HPLC-MS information to generate heatmaps of compounds monitored for subsequent data analysis was also available in the software. The system was evaluated with whole-body thin tissue sections from propranolol dosed rat. The hands-free operation of the system was demonstrated by creating heatmaps of the parent drug and its hydroxypropranolol glucuronide metabolites with 1 mm resolution in the areas of interest. The sample throughput was approximately 5 min/sample defined by the time needed for chromatographic separation. The spatial distributions of both the drug and its metabolites were consistent with previous studies employing other liquid extraction-based surface sampling methodologies.

  20. A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

    Science.gov (United States)

    Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

    2005-02-15

    A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

  1. Ciclosporine A asxay: RIA or HPLC, plasma or total blood

    International Nuclear Information System (INIS)

    Lapalus, P.; Garraffo, R.; Krebs, B.; Lapalus, F.

    1985-01-01

    The two methods now in force for ciclosporine A assay are radioimmunoassay (RIA) and high pressure liquid chromatography (HPLC) in various biological media (plasma, serum, total blood). The advantages and disadvantages of the two methods are presented [fr

  2. [HPLC characteristic fingerprints of sedi linearis herba and sedi herba].

    Science.gov (United States)

    Lu, Lan-Qing; Mei, Qing; Wan, Ding-Rong; Yang, Xin-Zhou; Qiao, Shu; Zhao, Yu-Dan

    2014-04-01

    To study HPLC characteristic fingerprint of Sedum lineare from different harvest periods, and to compare with its related species Sedum sarmentosum. The HPLC fingerprints of Sedum lineare from different collecting periods were established and compared with Sedum sarmentosum by the same detection method. Hyperin, isoquercitrin and astragaloside were identified from the HPLC fingerprint of Sedum lineare. The fingerprint of Sedum lineare growing in the same area but different environment were basically identical; while there were remarkable differences of Sedum lineare growing in the same place but from different harvest periods, with the area of most common peaks changing from little to great, and slightly different peak number. The HPLC fingerprint of the two Sedum species had four common peaks, but could be distinguished from each other. The optimal harvest period of these two species should be full-bloom stage. The established method can provide reference for identification and quality analysis of Sedum lineare.

  3. Development of Reverse-Phase HPLC Method for Simultaneous ...

    African Journals Online (AJOL)

    Erah

    Purpose: To develop a simple, sensitive and rapid reverse phase HPLC method for the simultaneous analysis of metoprolol succinate and hydrochlorothiazide in a solid dosage form. Methods: The .... Extraction was carried out three times with.

  4. A case report of percutaneous endoscopic gastrostomy left-side gastropexy to resolve a recurrent gastric dilatation in a dog previously treated with right-side gastropexy for gastric dilatation volvulus.

    Science.gov (United States)

    Spinella, Giuseppe; Cinti, Filippo; Pietra, Marco; Capitani, Ombretta; Valentini, Simona

    2014-12-01

    A 6-year-old, large-breed, female dog was evaluated for gastric dilatation (GD). The dog was affected by GD volvulus, which had been surgically treated with gastric derotation and right incisional gastropexy. Recurrence of GD appeared 36 hours after surgery. The dilatation was immediately treated with an orogastric probe but still recurred 4 times. Therefore, a left-side gastropexy by percutaneous endoscopic gastrostomy (PEG) was performed to prevent intermittent GD. After PEG tube placement, the patient recovered rapidly without side effects. Several techniques of gastropexy have been described as a prophylactic method for gastric dilatation volvulus, but to the authors' knowledge, this is the first report of left-sided PEG gastropexy performed in a case of canine GD recurrence after an incisional right gastropexy. Copyright © 2015 Elsevier Inc. All rights reserved.

  5. Underestimation of Severity of Previous Whiplash Injuries

    Science.gov (United States)

    Naqui, SZH; Lovell, SJ; Lovell, ME

    2008-01-01

    INTRODUCTION We noted a report that more significant symptoms may be expressed after second whiplash injuries by a suggested cumulative effect, including degeneration. We wondered if patients were underestimating the severity of their earlier injury. PATIENTS AND METHODS We studied recent medicolegal reports, to assess subjects with a second whiplash injury. They had been asked whether their earlier injury was worse, the same or lesser in severity. RESULTS From the study cohort, 101 patients (87%) felt that they had fully recovered from their first injury and 15 (13%) had not. Seventy-six subjects considered their first injury of lesser severity, 24 worse and 16 the same. Of the 24 that felt the violence of their first accident was worse, only 8 had worse symptoms, and 16 felt their symptoms were mainly the same or less than their symptoms from their second injury. Statistical analysis of the data revealed that the proportion of those claiming a difference who said the previous injury was lesser was 76% (95% CI 66–84%). The observed proportion with a lesser injury was considerably higher than the 50% anticipated. CONCLUSIONS We feel that subjects may underestimate the severity of an earlier injury and associated symptoms. Reasons for this may include secondary gain rather than any proposed cumulative effect. PMID:18201501

  6. Quality of life with palbociclib plus fulvestrant in previously treated hormone receptor-positive, HER2-negative metastatic breast cancer: patient-reported outcomes from the PALOMA-3 trial.

    Science.gov (United States)

    Harbeck, N; Iyer, S; Turner, N; Cristofanilli, M; Ro, J; André, F; Loi, S; Verma, S; Iwata, H; Bhattacharyya, H; Puyana Theall, K; Bartlett, C H; Loibl, S

    2016-06-01

    In the PALOMA-3 study, palbociclib plus fulvestrant demonstrated improved progression-free survival compared with fulvestrant plus placebo in hormone receptor-positive, HER2- endocrine-resistant metastatic breast cancer (MBC). This analysis compared patient-reported outcomes (PROs) between the two treatment groups. Patients were randomized 2 : 1 to receive palbociclib 125 mg/day orally for 3 weeks followed by 1 week off (n = 347) plus fulvestrant (500 mg i.m. per standard of care) or placebo plus fulvestrant (n = 174). PROs were assessed on day 1 of cycles 1-4 and of every other subsequent cycle starting with cycle 6 using the EORTC QLQ-C30 and its breast cancer module, QLQ-BR23. High scores (range 0-100) could indicate better functioning/quality of life (QoL) or worse symptom severity. Repeated-measures mixed-effect analyses were carried out to compare on-treatment overall scores and changes from baseline between treatment groups while controlling for baseline. Between-group comparisons of time to deterioration in global QoL and pain were made using an unstratified log-rank test and Cox proportional hazards model. Questionnaire completion rates were high at baseline and during treatment (from baseline to cycle 14, ≥95.8% in each group completed ≥1 question on the EORTC QLQ-C30). On treatment, estimated overall global QoL scores significantly favored the palbociclib plus fulvestrant group [66.1, 95% confidence interval (CI) 64.5-67.7 versus 63.0, 95% CI 60.6-65.3; P = 0.0313]. Significantly greater improvement from baseline in pain was also observed in this group (-3.3, 95% CI -5.1 to -1.5 versus 2.0, 95% CI -0.6 to 4.6; P = 0.0011). No significant differences were observed for other QLQ-BR23 functioning domains, breast or arm symptoms. Treatment with palbociclib plus fulvestrant significantly delayed deterioration in global QoL (P < 0.025) and pain (P < 0.001) compared with fulvestrant alone. Palbociclib plus fulvestrant allowed patients to maintain good Qo

  7. Separation and Simultaneous Determination of 14 Fungicides with the Combination of Multi-Analyte Methods and HPLC Detection

    Energy Technology Data Exchange (ETDEWEB)

    Canping, Pan [Department of Applied Chemistry, China Agricultural University, Beijing (China)

    2009-07-15

    The separation and simultaneous HPLC-MS determination for a series of fungicide products is reported. Multi-analyte methods were applied on a Chromolith RP-18e monolithic column having low resistance and enabling high flow rates and short analysis time at very good separation power. Details and analytical conditions are described with chromatograms illustrating the results and work done. (author)

  8. A systematic approach to the accurate quantification of selenium in serum selenoalbumin by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Jitaru, Petru; Goenaga-Infante, Heidi; Vaslin-Reimann, Sophie; Fisicaro, Paola

    2010-01-01

    In this paper, two different methods are for the first time systematically compared for the determination of selenium in human serum selenoalbumin (SeAlb). Firstly, SeAlb was enzymatically hydrolyzed and the resulting selenomethionine (SeMet) was quantified using species-specific isotope dilution (SSID) with reversed phase-HPLC (RP-HPLC) hyphenated to (collision/reaction cell) inductively coupled plasma-quadrupole mass spectrometry (CRC ICP-QMS). In order to assess the enzymatic hydrolysis yield, SeAlb was determined as an intact protein by affinity-HPLC (AF-HPLC) coupled to CRC ICP-QMS. Using this approach, glutathione peroxidase (GPx) and selenoprotein P (SelP) (the two selenoproteins present in serum) were also determined within the same chromatographic run. The levels of selenium associated with SeAlb in three serum materials, namely BCR-637, Seronorm level 1 and Seronorm level 2, obtained using both methods were in a good agreement. Verification of the absence of free SeMet, which interferes with the SeAlb determination (down to the amino acid level), in such materials was addressed by analyzing the fraction of GPx, partially purified by AF-HPLC, using RP-HPLC (GPx only) and size exclusion-HPLC (SE-HPLC) coupled to CRC ICP-QMS. The latter methodology was also used for the investigation of the presence of selenium species other than the selenoproteins in the (AF-HPLC) SelP and SeAlb fractions; the same selenium peaks were detected in both control and BCR-637 serum with a difference in age of ca. 12 years. It is also for the first time that the concentrations of selenium associated with SeAlb, GPx and SelP species in such commercially available serums (only certified or having indicative levels of total selenium content) are reported. Such indicative values can be used for reference purposes in future validation of speciation methods for selenium in human serum and/or inter-laboratory comparisons.

  9. A systematic approach to the accurate quantification of selenium in serum selenoalbumin by HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Jitaru, Petru, E-mail: Petru.Jitaru@lne.fr [Laboratoire National de Metrologie et d' Essais (LNE), Department of Biomedical and Inorganic Chemistry, 1 rue Gaston Boissier, 75015 Paris (France); Goenaga-Infante, Heidi [LGC Limited, Queens Road, Teddington, TW11 OLY, Middlesex (United Kingdom); Vaslin-Reimann, Sophie; Fisicaro, Paola [Laboratoire National de Metrologie et d' Essais (LNE), Department of Biomedical and Inorganic Chemistry, 1 rue Gaston Boissier, 75015 Paris (France)

    2010-01-11

    In this paper, two different methods are for the first time systematically compared for the determination of selenium in human serum selenoalbumin (SeAlb). Firstly, SeAlb was enzymatically hydrolyzed and the resulting selenomethionine (SeMet) was quantified using species-specific isotope dilution (SSID) with reversed phase-HPLC (RP-HPLC) hyphenated to (collision/reaction cell) inductively coupled plasma-quadrupole mass spectrometry (CRC ICP-QMS). In order to assess the enzymatic hydrolysis yield, SeAlb was determined as an intact protein by affinity-HPLC (AF-HPLC) coupled to CRC ICP-QMS. Using this approach, glutathione peroxidase (GPx) and selenoprotein P (SelP) (the two selenoproteins present in serum) were also determined within the same chromatographic run. The levels of selenium associated with SeAlb in three serum materials, namely BCR-637, Seronorm level 1 and Seronorm level 2, obtained using both methods were in a good agreement. Verification of the absence of free SeMet, which interferes with the SeAlb determination (down to the amino acid level), in such materials was addressed by analyzing the fraction of GPx, partially purified by AF-HPLC, using RP-HPLC (GPx only) and size exclusion-HPLC (SE-HPLC) coupled to CRC ICP-QMS. The latter methodology was also used for the investigation of the presence of selenium species other than the selenoproteins in the (AF-HPLC) SelP and SeAlb fractions; the same selenium peaks were detected in both control and BCR-637 serum with a difference in age of ca. 12 years. It is also for the first time that the concentrations of selenium associated with SeAlb, GPx and SelP species in such commercially available serums (only certified or having indicative levels of total selenium content) are reported. Such indicative values can be used for reference purposes in future validation of speciation methods for selenium in human serum and/or inter-laboratory comparisons.

  10. Single sample extraction and HPLC processing for quantification of NAD and NADH levels in Saccharomyces cerevisiae

    Energy Technology Data Exchange (ETDEWEB)

    Sporty, J; Kabir, M M; Turteltaub, K; Ognibene, T; Lin, S; Bench, G

    2008-01-10

    A robust redox extraction protocol for quantitative and reproducible metabolite isolation and recovery has been developed for simultaneous measurement of nicotinamide adenine dinucleotide (NAD) and its reduced form, NADH, from Saccharomyces cerevisiae. Following culture in liquid media, approximately 10{sup 8} yeast cells were harvested by centrifugation and then lysed under non-oxidizing conditions by bead blasting in ice-cold, nitrogen-saturated 50-mM ammonium acetate. To enable protein denaturation, ice cold nitrogen-saturated CH{sub 3}CN + 50-mM ammonium acetate (3:1; v:v) was added to the cell lysates. After sample centrifugation to pellet precipitated proteins, organic solvent removal was performed on supernatants by chloroform extraction. The remaining aqueous phase was dried and resuspended in 50-mM ammonium acetate. NAD and NADH were separated by HPLC and quantified using UV-VIS absorbance detection. Applicability of this procedure for quantifying NAD and NADH levels was evaluated by culturing yeast under normal (2% glucose) and calorie restricted (0.5% glucose) conditions. NAD and NADH contents are similar to previously reported levels in yeast obtained using enzymatic assays performed separately on acid (for NAD) and alkali (for NADH) extracts. Results demonstrate that it is possible to perform a single preparation to reliably and robustly quantitate both NAD and NADH contents in the same sample. Robustness of the protocol suggests it will be (1) applicable to quantification of these metabolites in mammalian and bacterial cell cultures; and (2) amenable to isotope labeling strategies to determine the relative contribution of specific metabolic pathways to total NAD and NADH levels in cell cultures.

  11. Sensitive measurement of positron emitters eluted from HPLC

    International Nuclear Information System (INIS)

    Takei, Makoto; Kida, Takayo; Suzuki, Kazutoshi

    2001-01-01

    For sensitive analysis of the radioactive-metabolite in human PET, a radio-HPLC system coupled to a newly designed positron detector was constructed. The detector had the advantages of low noise level (1.7±1.0 cpm) and high sensitivity (32±1%) due to coincidence counting and large BGO crystals. Furthermore, the detector was easy to move, since a pair of the BGO housings coupled to photomultipliers was effectively arranged in parallel and a HPLC cell with different volume could be inserted between the BGO housing. This radio-HPLC system was useful for analyzing samples with low radioactivity. It was applied to the measurement of [ 11 C]FLB457 in plasma, having high affinity and high selectivity with dopamine D2 receptors. Extremely low radioactivity of [ 11 C]FLB457 (2500 dpm) could be analyzed by using the radio-HPLC system. The performance of this detector was compared with those of commercially available systems that had been used as sensitive detectors for HPLC

  12. [Determination of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla by HPLC].

    Science.gov (United States)

    Yang, Xiu-Juan; Hong, Yan-Long; Wu, Fei; Ruan, Ke-Feng; Feng, Yi

    2013-03-01

    To explore an HPLC method for determination of rhnchophylline and isorhnchophylline in Uncaria rhnchophylla. An HPLC method has been developed for determination of rhnchophylline and isorhnchophylline. The transformation of rhnchophylline and isorhnchophylline after heating was also studied by HPLC-ESI-MS. Good linearities of rhynchophylline and isorhynchophylline were 0.064-5.100, 0.064-5.110 mg, respectively. The average recoveries were from 87.51% to 88.83% for rhynchophylline and from 107.9% to 113.9% for isorhynchophylline. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 12.60% and 40.00% in the reflux extraction procedure, respectively. While in the ultrasonic extraction procedure, the average recoveries of rhynchophylline and isorhynchophylline was from 99.48% to 103.2% and from 97.00% to 99.59%, resepectively. The recoveries of rhynchophylline and isorhnchophylline reference solutions after extraction were 47.08% and 51.03%, respectively. The unqualified recovery could be elucidated by HPLC-ESI-MS analysis, indicating that trhynchophylline could be transformed mostly into isorhynchophylline and a little amount of unkown composition, while isorhynchophylline could be transformed into rhynchophylline isocorynoxeine, corynoxeine and 22-O-beta-D-glucopyranosyl isocorynoxeinic acid during the extraction procedure. Ultrasonic extraction procedure was more sutble for HPLC determination of the content of rhynchophylline and isorhynchophylline in U. rhnchophylla, however, the recovery problems should be paid attention to when it comes to the determination.

  13. Identification and quantitation of asparagine and citrulline using high-performance liquid chromatography (HPLC).

    Science.gov (United States)

    Bai, Cheng; Reilly, Charles C; Wood, Bruce W

    2007-03-28

    High-performance liquid chromatography (HPLC) analysis was used for identification of two problematic ureides, asparagine and citrulline. We report here a technique that takes advantage of the predictable delay in retention time of the co-asparagine/citrulline peak to enable both qualitative and quantitative analysis of asparagine and citrulline using the Platinum EPS reverse-phase C18 column (Alltech Associates). Asparagine alone is eluted earlier than citrulline alone, but when both of them are present in biological samples they may co-elute. HPLC retention times for asparagine and citrulline were influenced by other ureides in the mixture. We found that at various asparagines and citrulline ratios [= 3:1, 1:1, and 1:3; corresponding to 75:25, 50:50, and 25:75 (microMol ml(-1)/microMol ml(-1))], the resulting peak exhibited different retention times. Adjustment of ureide ratios as internal standards enables peak identification and quantification. Both chemicals were quantified in xylem sap samples of pecan [Carya illinoinensis (Wangenh.) K. Koch] trees. Analysis revealed that tree nickel nutrition status affects relative concentrations of Urea Cycle intermediates, asparagine and citrulline, present in sap. Consequently, we concluded that the HPLC methods are presented to enable qualitative and quantitative analysis of these metabolically important ureides.

  14. Identification and Quantitation of Asparagine and Citrulline Using High-Performance Liquid Chromatography (HPLC

    Directory of Open Access Journals (Sweden)

    Cheng Bai

    2007-01-01

    Full Text Available High-performance liquid chromatography (HPLC analysis was used for identification of two problematic ureides, asparagine and citrulline. We report here a technique that takes advantage of the predictable delay in retention time of the co-asparagine/citrulline peak to enable both qualitative and quantitative analysis of asparagine and citrulline using the Platinum EPS reverse-phase C18 column (Alltech Associates. Asparagine alone is eluted earlier than citrulline alone, but when both of them are present in biological samples they may co-elute. HPLC retention times for asparagine and citrulline were influenced by other ureides in the mixture. We found that at various asparagines and citrulline ratios [= 3:1, 1:1, and 1:3; corresponding to 75:25, 50:50, and 25:75 (μMol ml–1/μMol ml–1], the resulting peak exhibited different retention times. Adjustment of ureide ratios as internal standards enables peak identification and quantification. Both chemicals were quantified in xylem sap samples of pecan [Carya illinoinensis (Wangenh. K. Koch] trees. Analysis revealed that tree nickel nutrition status affects relative concentrations of Urea Cycle intermediates, asparagine and citrulline, present in sap. Consequently, we concluded that the HPLC methods are presented to enable qualitative and quantitative analysis of these metabolically important ureides.

  15. Surface-enhanced Raman detection of RNA and DNA bases following flow-injection analysis or HPLC separation

    Science.gov (United States)

    Cotton, Therese M.; Sheng, Rong-Sheng; Ni, Fan

    1990-11-01

    The goal of this study is to develop Surface-enhanced Raman scattering (SERS) detection methods for flow injection analysis (FIA) and high performance liquid chromatography (HPLC). Nucleic acid bases have been chosen for analysis because of their importance in life processes. The advantages to the use of SERS-based detection include its sensitivity, specificity and versatility. With the development of improved methodology, the detection limits should be comparable to UV spectroscopy. However, the specificity is considerably superior to that obtained with electronic spectroscopy in that the Raman spectrum provides a molecular fingerprint of the individual analytes. Raman spectroscopy is very versatile: aqueous samples, gases and solids can be analyzed with equal facility. The results presented here demonstrate that SERS can be used as a detection method for both FIA and HPLC detection. In the following experiments Ag sols have been used as the active substrate. The effect of various parameters such as temperature, pH, flow rate, and the nature of the interface between the HPLC system and the Raman spectrometer have been examined. One of the most significant findings is that the temperature of the Ag sol/HPLC effluent mixture has a dramatic effect on the SERS intensities. This effect is a result of increased colloid aggregation at higher temperatures. Aggregation is known to produce greater enhancement in SERS and proceeds much more rapidly at elevated temperatures. An increase in the temperature of the Ag sol enables SERS detection under flowing conditions and in real time. This is a substantial improvement over many of the previous attempts to interface SERS detection to FIA or HPLC. In most of the previous studies, it was necessary to stop the flow as the analyte eluted from the chromatogram and measure the SERS spectra under static conditions.

  16. Assessment of radiochemical purity of [{sup 18}F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z., E-mail: radiofarmacoscdtn@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Producao de Radiofarmacos

    2011-07-01

    The quality control of [{sup 18}F]fludeoxyglucose ({sup 18}FDG) has received attention due to its increasing clinical use. Although the quality requirements of {sup 18}FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of {sup 18}FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. {sup 18}FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of {sup 18}FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of {sup 18}FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of {sup 18}FDG, considering operational conditions of our laboratory. (author)

  17. Glycyrrhiza glabra HPLC fractions: identification of Aldehydo Isoophiopogonone and Liquirtigenin having activity against multidrug resistant bacteria.

    Science.gov (United States)

    Rahman, Hazir; Khan, Ilyas; Hussain, Anwar; Shahat, Abdelaaty Abdelaziz; Tawab, Abdul; Qasim, Muhammad; Adnan, Muhammad; Al-Said, Mansour S; Ullah, Riaz; Khan, Shahid Niaz

    2018-05-02

    Medicinal plants have been founded as traditional herbal medicine worldwide. Most of the plant's therapeutic properties are due to the presence of secondary metabolites such as alkaloids, glycosides, tannins and volatile oil. The present investigation analyzed the High-Pressure Liquid Chromatography (HPLC) fractions of Glycyrrhiza glabra (Aqueous, Chloroform, Ethanol and Hexane) against multidrug resistant human bacterial pathogens (Escherichia coli, Acinetobacter baumannii, Staphylococcus aureus and Pseudomonas aeruginosa). All the fractions showed antibacterial activity, were subjected to LC MS/MS analysis for identification of bioactive compounds. Among total HPLC fractions of G. glabra (n = 20), three HPLC fractions showed potential activity against multidrug resistant (MDR) bacterial isolates. Fraction 1 (F1) of aqueous extracts, showed activity against A. baumannii (15 ± 0.5 mm). F4 from hexane extract of G. glabra showed activity against S. aureus (10 ± 0.2 mm). However, F2 from ethanol extract exhibited activity against S. aureus (10 ± 0.3 mm). These active fractions were further processed by LC MS/MS analysis for the identification of compounds. Ellagic acid was identified in the F1 of aqueous extract while 6-aldehydo-isoophiopogonone was present in F4 of hexane extract. Similarly, Liquirtigenin was identified in F2 of ethanol. Glycyrrhiza glabra extracts HPLC fractions showed anti-MDR activity. Three bioactive compounds were identified in the study. 6-aldehydo-isoophiopogonone and Liquirtigenin were for the first time reported in G. glabra. Further characterization of the identified compounds will be helpful for possible therapeutic uses against infectious diseases caused by multidrug resistant bacteria.

  18. Assessment of radiochemical purity of [18F]fludeoxyglucose by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Lacerda, Aline E.; Silva, Juliana B.; Silveira, Marina B.; Ferreira, Soraya Z.

    2011-01-01

    The quality control of [ 18 F]fludeoxyglucose ( 18 FDG) has received attention due to its increasing clinical use. Although the quality requirements of 18 FDG are established in various pharmacopoeia, the suitability of all testing methods used should be verified under actual conditions of use and documented. The aim of this study was to develop a high pressure liquid chromatography (HPLC) method for radiochemical purity evaluation of 18 FDG, based on pharmacopoeia references, and to verify its suitability for routine quality control in our centre. HPLC analysis was performed with an Agilent HPLC. 18 FDG and impurities were separated on an anion-exchange column by isocratic elution with 0.1 M NaOH as the mobile phase. Detection was accomplished with refractive index and NaI (Tl) scintillation detectors. The flow rate of the mobile phase was set at 0.8 mL/min and the column temperature was kept at 35 deg C. Specificity, linearity, precision and robustness were assessed to verify if the method was adequate for its intended purpose. Retention time of 18 FDG was not affected by the presence of other components of the formulation and a good peak resolution was achieved. The analytical curve of 18 FDG was linear, with a correlation coefficient value of 0.9995. Intraday repeatable precision, reported as the relative standard deviation, was 0.11%. Analytical procedure remained unaffected by small variations in mobile phase flow rate. Results evidenced that HPLC is suitable for radiochemical purity evaluation of 18 FDG, considering operational conditions of our laboratory. (author)

  19. Seizure is a rare presentation for acute hemolysis due to G6PD deficiency. We report a previously healthy boy who presented initially with seizure and cyanosis and subsequently acute hemolysis, due to glucose-6-phosphate dehydrogenase deficiency (G6PD) an

    OpenAIRE

    Afshin FAYYAZI; Ali KHAJEH; Hosein ESFAHANI

    2012-01-01

    Seizure is a rare presentation for acute hemolysis due to G6PD deficiency. We report a previously healthy boy who presented initially with seizure and cyanosis and subsequently acute hemolysis, due to glucose-6-phosphate dehydrogenase deficiency (G6PD) and probably secondary methemoglobinemia, following the ingestion of fava beans.

  20. Assay of flavonoid aglycones from the species of genus Sideritis (Lamiaceae) from Macedonia with HPLC-UV DAD.

    Science.gov (United States)

    Janeska, Bisera; Stefova, Marina; Alipieva, Kalina

    2007-09-01

    Flavonoids obtained from Sideritis species (Lamiaceae), S. raeseri and S. scardica, grown in Macedonia were studied. Qualitative and quantitative analyses of the flavonoid aglycones were performed using high-performance liquid chromatography (HPLC) with a UV diode array detector. Extracts were prepared by acid hydrolysis in acetone, re-extraction in ethyl acetate and evaporation to dryness; the residue dissolved in methanol was subjected to HPLC analysis.Isoscutellarein, chryseriol and apigenin were identified in the extracts. Also, a 4'-methyl ether derivative of isoscutellarein was found, together with hypolaetin and its methyl ether derivative, which were identified according to previously isolated glycosides and literature data. Quantitation was performed using calibration with apigenin.According to this screening analysis, the samples of the genus Sideritis from Macedonia are rich in polyhydroxy flavones and analogous with the previously studied Mediterranean Sideritis species from the Ibero-North African and Greek Sideritis species with respect to the presence of 8-OH flavones and their derivatives.

  1. The influence of previous low back trouble, general health, and working conditions on future sick-listing because of low back trouble. A 15-year follow-up study of risk indicators for self-reported sick-listing caused by low back trouble.

    Science.gov (United States)

    Müller, C F; Monrad, T; Biering-Sørensen, F; Darre, E; Deis, A; Kryger, P

    1999-08-01

    A 15-year follow-up study. To find risk indicators for self-reported sick-listing because of low back trouble and to evaluate which variables were the most important indicators of work incapacity resulting from low back trouble during the follow-up period of 15 years. The initial data were obtained from a health survey conducted in a general population from the Municipality of Glostrup, Denmark. The follow-up data included information from the Central Person Register, the Early Retirement Pension Register, and a postal questionnaire regarding self-reported sick-listing because of low back trouble. An epidemiologic study, in which logistic regression analyses were used for evaluation of the data. The model used consisted of the variable in question, age, gender, and previous experience of low back trouble, along with interactions. It was found that 22 of 37 variables were risk indicators for later self-reported sick-listing because of low back trouble during the preceding year or the 7 years before the date of follow-up evaluation. In analyzing the most significant variables simultaneously, it was found that information from the initial investigation about sick-listing in general during the previous 10 years, sciatic pain, use of analgesics for low back trouble, previous sick-listing because of low back trouble, and occupation were the most important risk indicators for self-reported work incapacity resulting from low back trouble during the follow-up period of 15 years. Findings showed that the strongest prognostic indicators of later sick-listing because of low back trouble involve information from the person about previous sick-listing behavior in general and previous experience of low back trouble episodes, especially if these had been accompanied by sciatic pain, use of analgesics, or previous low back trouble sick-listing.

  2. Quantitation of radiolabeled compounds eluting from the HPLC system

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1982-01-01

    Three techniques are compared for the quantitation of various radiolabeled compounds eluting in the high performance liquid chromatography system. The first technique requires fraction-collecting the effluent from the HPLC, removing an aliquot to scintillation vials, and counting each fraction in a liquid scintillation counter. The second uses direct interface of the HPLC effluent to a flow-through radioactivity detector. The third involves quantitation of various radiolabeled compounds (proteins, steroids, and nucleotides) by splitting the effluent from the HPLC with an electronic steam splitter, thus diverting a present portion to the fraction collector for further chemical characterization and the remainder to the radioactivity flow detector for direct quantitation. A direct comparison of the chromatograms and the radioactivity counting efficiencies of these three techniques is presented

  3. A hybrid FIA/HPLC system incorporating monolithic column chromatography

    International Nuclear Information System (INIS)

    Adcock, Jacqui L.; Francis, Paul S.; Agg, Kent M.; Marshall, Graham D.; Barnett, Neil W.

    2007-01-01

    We have combined the generation of solvent gradients using milliGAT pumps, chromatographic separations with monolithic columns and chemiluminescence detection in an instrument manifold that approaches the automation and separation efficiency of HPLC, whilst maintaining the positive attributes of flow injection analysis (FIA), such as manifold versatility, speed of analysis and portability. As preliminary demonstrations of this hybrid FIA/HPLC system, we have determined six opiate alkaloids (morphine, pseudomorphine, codeine, oripavine, ethylmorphine and thebaine) and four biogenic amines (vanilmandelic acid, serotonin, 5-hydroxyindole-3-acetic acid and homovanillic acid) in human urine, using tris(2,2'-bipyridyl)ruthenium(III) and acidic potassium permanganate chemiluminescence detection

  4. Forensic intoxication with clobazam: HPLC/DAD/MSD analysis.

    Science.gov (United States)

    Proença, Paula; Teixeira, Helena; Pinheiro, João; Marques, Estela P; Vieira, Duarte Nuno

    2004-07-16

    Clobazam (Castillium, Urbanil), a benzodiazepine often used as an anxiolytic and in the treatment of epilepsy, is considered a relatively safe drug. The authors present a fatal case with a 49-year-old female, found dead at home. She had been undergoing psychiatric treatment and was a chronic alcoholic. The autopsy findings were unremarkable, except for multivisceral congestion, steatosis and a small piece of a plastic blister pack in the stomach. Bronchopneumonia, bronchitis and bronchiolitis were also diagnosed. Anhigh-performance liquid chromatography (HPLC)/diode array detector (DAD)/mass spectrometry detection (MSD) with electrospray method was developed in order to detect, confirm and quantify clobazam in the post-mortem samples. In the chromatographic separation, a reversed-phase column C18 (2.1 x 150 mm, 3.5 microm) was used with a mobile phase of methanol and water, at a 0.25 ml/min flow rate. Carbonate buffer (pH 10.5) and 20 microl of prazepam (100 microg/ml) as internal standard were added to the samples. A simple and reliable liquid-liquid extraction method for the determination of clobazam in post-mortem samples was described. Calibration curves for clobazam were performed in blood, achieving linearity between 0.01 and 10 microg/ml and a detection limit of 1.0 ng/ml. The clobazam concentration found in post-mortem blood was 3.9 microg/ml, higher than the reported therapeutic concentration (0.1-0.4 microg/ml). The simultaneous acquisition by photodiode array detection and mass spectrometry detection results allowed benzodiazepines to be identified with sufficient certainty. An examination of all the available information suggested that death resulted from respiratory depression due to clobazam toxicity.

  5. Chemical fingerprinting and quantitative analysis of a Panax notoginseng preparation using HPLC-UV and HPLC-MS

    Directory of Open Access Journals (Sweden)

    Shao Qing

    2011-02-01

    Full Text Available Abstract Background Xuesaitong (XST injection, consisting of total saponins from Panax notoginseng, was widely used for the treatment of cardio- and cerebro-vascular diseases in China. This study develops a simple and global quality evaluation method for the quality control of XST. Methods High performance liquid chromatography-ultraviolet detection (HPLC-UV was used to identify and quantify the chromatographic fingerprints of the XST injection. Characteristic common peaks were identified using HPLC with photo diode array detection/electrospray ionization tandem mass spectrometry (HPLC-PDA/ESI-MSn. Results Representative fingerprints from ten batches of samples showed 27 'common saponins' all of which were identified and quantified using ten reference saponins. Conclusion Chemical fingerprinting and quantitative analysis identified most of the common saponins for the quality control of P. notoginseng products such as the XST injection.

  6. Preoperative screening: value of previous tests.

    Science.gov (United States)

    Macpherson, D S; Snow, R; Lofgren, R P

    1990-12-15

    To determine the frequency of tests done in the year before elective surgery that might substitute for preoperative screening tests and to determine the frequency of test results that change from a normal value to a value likely to alter perioperative management. Retrospective cohort analysis of computerized laboratory data (complete blood count, sodium, potassium, and creatinine levels, prothrombin time, and partial thromboplastin time). Urban tertiary care Veterans Affairs Hospital. Consecutive sample of 1109 patients who had elective surgery in 1988. At admission, 7549 preoperative tests were done, 47% of which duplicated tests performed in the previous year. Of 3096 previous results that were normal as defined by hospital reference range and done closest to the time of but before admission (median interval, 2 months), 13 (0.4%; 95% CI, 0.2% to 0.7%), repeat values were outside a range considered acceptable for surgery. Most of the abnormalities were predictable from the patient's history, and most were not noted in the medical record. Of 461 previous tests that were abnormal, 78 (17%; CI, 13% to 20%) repeat values at admission were outside a range considered acceptable for surgery (P less than 0.001, frequency of clinically important abnormalities of patients with normal previous results with those with abnormal previous results). Physicians evaluating patients preoperatively could safely substitute the previous test results analyzed in this study for preoperative screening tests if the previous tests are normal and no obvious indication for retesting is present.

  7. Automatic electromagnetic valve for previous vacuum

    International Nuclear Information System (INIS)

    Granados, C. E.; Martin, F.

    1959-01-01

    A valve which permits the maintenance of an installation vacuum when electric current fails is described. It also lets the air in the previous vacuum bomb to prevent the oil ascending in the vacuum tubes. (Author)

  8. Characterization of polymer monolithic stationary phases for capillary HPLC

    Czech Academy of Sciences Publication Activity Database

    Moravcová, D.; Jandera, P.; Urban, J.; Planeta, Josef

    2003-01-01

    Roč. 26, č. 11 (2003), s. 1005-1016 ISSN 1615-9306 R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4031919; CEZ:MSM 253100002 Keywords : monolithic column s * capillary HPLC * column testing Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.108, year: 2003

  9. Validated RP-HPLC Method for Quantification of Phenolic ...

    African Journals Online (AJOL)

    Purpose: To evaluate the total phenolic content and antioxidant potential of the methanol extracts of aerial parts and roots of Thymus sipyleus Boiss and also to determine some phenolic compounds using a newly developed and validated reversed phase high performance liquid chromatography (RP-HPLC) method.

  10. Rapid and Reliable HPLC Method for the Determination of Vitamin ...

    African Journals Online (AJOL)

    Purpose: To develop and validate an accurate, sensitive and reproducible high performance liquid chromatographic (HPLC) method for the quantitation of vitamin C in pharmaceutical samples. Method: The drug and the standard were eluted from Superspher RP-18 (250 mm x 4.6 mm, 10ìm particle size) at 20 0C.

  11. A Simple HPLC Bioanalytical Method for the Determination of ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, accurate, and precise high performance chromatography (HPLC) method with spectrophotometric detection for the determination of doxorubicin hydrochloride in rat plasma. Methods: Doxorubicin hydrochloride and daunorubicin hydrochloride (internal standard, IS) were separated on a C18 ...

  12. A Stability Indicating HPLC Method for the Determination of ...

    African Journals Online (AJOL)

    Erah

    stability indicating reverse phase HPLC method for estimating meloxicam (MLX) in bulk ... acetonitrile-water-glacial acetic acid [55:40:5 (% v/v)] at a flow rate of 1ml/min and detection wavelength .... pore and degassed before use. ... determined to assess the effect of small but ... deviation, the standard error of slope, and the.

  13. Separation of complex oligosaccharides from wort and beer using HPLC

    Czech Academy of Sciences Publication Activity Database

    Cabálková, Jana; Bobálová, Janette

    2008-01-01

    Roč. 102, č. 15 (2008), s608-s609 ISSN 1803-2389. [Meeting on Chemistry and Life /4./. Brno, 09.09.2008-11.09.2008] R&D Projects: GA MŠk 2B06037 Institutional research plan: CEZ:AV0Z40310501 Keywords : oligosacharides * beer * HPLC Subject RIV: CB - Analytical Chemistry, Separation

  14. SCREENING CORD BLOOD FOR HEMOGLOBINOPATHIES AND THALASSEMIA BY HPLC

    NARCIS (Netherlands)

    VANDERDIJS, FPL; VANDENBERG, GA; SCHERMER, JG; MUSKIET, FD; LANDMAN, H; MUSKIET, FAJ

    We evaluated the use of an HPLC method for screening hemoglobins in cord blood. We studied the genotype frequencies of the structural hemoglobin variants HbS and HbC and the synthesis variants alpha- and beta+-thalassemia in babies born on Curacao. During three months, 67.2% of all (748) newborns

  15. Chiral HPLC and physical characterisation of orthoconic antiferroelectric liquid crystals

    Czech Academy of Sciences Publication Activity Database

    Vojtylová, Terézia; Żurowska, M.; Milewska, K.; Hamplová, Věra; Sýkora, D.

    2016-01-01

    Roč. 43, č. 9 (2016), s. 1244-1250 ISSN 0267-8292 R&D Projects: GA MŠk(CZ) LD14007; GA ČR GA15-02843S Institutional support: RVO:68378271 Keywords : liquid crystals * chiral HPLC * orthoconic antiferroelectric LC Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.661, year: 2016

  16. Methods and applications of HPLC-AMS (WBio 5)

    International Nuclear Information System (INIS)

    Bucholz, B A; Clifford, A J; Duecker, S R; Lin, Y; Vogel, J S

    1999-01-01

    Pharmacokinetics of physiologic doses of nutrients, pesticides, and herbicides can easily be traced in humans using a(sup 14)C-labelled compound. Basic kinetics can be monitored in blood or urine by measuring the elevation in the(sup 14)C content above the control predose tissue and converting to equivalents of the parent compound. High Performance Liquid Chromatography (HPLC) is an excellent method for the chemical separation of complex mixtures whose profiles afford estimation of biochemical pathways of metabolism. Compounds elute from the HPLC systems with characteristic retention times and can be collected in fractions that can then be graphitized for AMS measurement. Unknowns are identified by coelution with known standards and chemical tests that reveal functional groupings. Metabolites are quantified with the(sup 14)C signal. Thoroughly accounting for the carbon inventory in the LC solvents, ion-pairing agents, samples, and carriers adds some complexity to the analysis. In most cases the total carbon inventory is dominated by carrier. Baseline background and stability need to be carefully monitored. Limits of quantitation near 10 amol of(sup 14)C per HPLC fraction are typically achieved. Baselines are maintained by limiting injected(sup 14)C activity and lt;0.17 Bq (4.5 pCi) on the HPLC column

  17. HPLC quantification of phenolic content and assessment of ...

    African Journals Online (AJOL)

    omotayo

    2016-03-02

    Mar 2, 2016 ... detection (HPLC-DAD) fingerprinting of phenolic content. Furthermore, the .... Briefly, deionised water (0.5 ml) and 125 μl of Folin–Colcalteu reagent were added to ..... to be organ-specific and can leak from a damaged or an.

  18. Stability and oxidation products of hydrolysable tannins in basic conditions detected by HPLC/DAD-ESI/QTOF/MS.

    Science.gov (United States)

    Tuominen, Anu; Sundman, Terhi

    2013-01-01

    Hydrolysable tannins occur in plants that are used for food or medicine by humans or herbivores. Basic conditions can alter the structures of tannins, that is, the oxidation of phenolic groups can lead to the formation of toxic quinones. Previously, these labile quinones and other oxidation products have been studied with colorimetric or electron paramagnetic resonance methods, which give limited information about products. To study the stability and oxidation products of hydrolysable tannins in basic conditions using HPLC with a diode-array detector (DAD) combined with electrospray ionisation (ESI) and quadrupole time-of-flight (QTOF) MS. Three galloyl glucoses, four galloyl derivatives with different polyols and three ellagitannins were purified from plants. The incubation reactions of tannins were monitored by HPLC/DAD at five pH values and in reduced oxygen conditions. Reaction products were identified based on UV spectra and mass spectral fragmentation obtained with the high-resolution HPLC/DAD-ESI/QTOF/MS. The use of a base-resistant HPLC column enabled injections without the sample pre-treatment and thus detection of short-lived products. Hydrolysable tannins were unstable in basic conditions and half-lives were mostly less than 10 min at pH 10. Degradation rates were faster at pH 11 but slower at milder pH. The HPLC analyses revealed that various products were formed and identified to be the result of hydrolysis, deprotonation and oxidation. Interestingly, the main hydrolysis product was ellagic acid; it was also formed from galloyl glucoses that do not contain oxidatively coupled galloyl groups in their initial structures. HPLD/DAD-ESI/QTOF/MS was an efficient method for the identification of polyphenol oxidation products and showed how different pH conditions determine the fate of hydrolysable tannins. Copyright © 2013 John Wiley & Sons, Ltd.

  19. HPLC Method for Simultaneous Quantitative Detection of Quercetin and Curcuminoids in Traditional Chinese Medicines

    Directory of Open Access Journals (Sweden)

    Lee Fung Ang

    2014-12-01

    Full Text Available Objectives: Quercetin and curcuminoids are important bioactive compounds found in many herbs. Previously reported high performance liquid chromatography ultraviolet (HPLC-UV methods for the detection of quercetin and curcuminoids have several disadvantages, including unsatisfactory separation times and lack of validation according the standard guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. Methods: A rapid, specific, reversed phase, HPLC-UV method with an isocratic elution of acetonitrile and 2% v/v acetic acid (40% : 60% v/v (pH 2.6 at a flow rate of 1.3 mL/minutes, a column temperature of 35°C, and ultraviolet (UV detection at 370 nm was developed. The method was validated and applied to the quantification of different types of market available Chinese medicine extracts, pills and tablets. Results: The method allowed simultaneous determination of quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin in the concentration ranges of 0.00488 ─ 200 μg/mL, 0.625 ─ 320 μg/mL, 0.07813 ─ 320 μg/mL and 0.03906 ─ 320 μg/mL, respectively. The limits of detection and quantification, respectively, were 0.00488 and 0.03906 μg/mL for quercetin, 0.62500 and 2.50000 μg/mL for bisdemethoxycurcumin, 0.07813 and 0.31250 μg/mL for demethoxycurcumin, and 0.03906 and 0.07813 μg/mL for curcumin. The percent relative intra day standard deviation (% RSD values were 0.432 ─ 0.806 μg/mL, 0.576 ─ 0.723 μg/ mL, 0.635 ─ 0.752 μg/mL and 0.655 ─ 0.732 μg/mL for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and those for intra day precision were 0.323 ─ 0.968 μg/mL, 0.805 ─ 0.854 μg/mL, 0.078 ─ 0.844 μg/mL and 0.275 ─ 0.829 μg/mL, respectively. The intra day accuracies were 99.589% ─ 100.821%, 98.588% ─ 101.084%, 9.289% ─ 100.88%, and 98.292% ─ 101.022% for quercetin, bisdemethoxycurcumin

  20. HPLC method for simultaneous quantitative detection of quercetin and curcuminoids in traditional chinese medicines.

    Science.gov (United States)

    Ang, Lee Fung; Yam, Mun Fei; Fung, Yvonne Tan Tze; Kiang, Peh Kok; Darwin, Yusrida

    2014-12-01

    Quercetin and curcuminoids are important bioactive compounds found in many herbs. Previously reported high performance liquid chromatography ultraviolet (HPLC-UV) methods for the detection of quercetin and curcuminoids have several disadvantages, including unsatisfactory separation times and lack of validation according the standard guidelines of the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use. A rapid, specific, reversed phase, HPLC-UV method with an isocratic elution of acetonitrile and 2% v/v acetic acid (40% : 60% v/v) (pH 2.6) at a flow rate of 1.3 mL/minutes, a column temperature of 35°C, and ultraviolet (UV) detection at 370 nm was developed. The method was validated and applied to the quantification of different types of market available Chinese medicine extracts, pills and tablets. The method allowed simultaneous determination of quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin in the concentration ranges of 0.00488 ─ 200 μg/mL, 0.625 ─ 320 μg/mL, 0.07813 ─ 320 μg/mL and 0.03906 ─ 320 μg/mL, respectively. The limits of detection and quantification, respectively, were 0.00488 and 0.03906 μg/mL for quercetin, 0.62500 and 2.50000 μg/mL for bisdemethoxycurcumin, 0.07813 and 0.31250 μg/mL for demethoxycurcumin, and 0.03906 and 0.07813 μg/mL for curcumin. The percent relative intra day standard deviation (% RSD) values were 0.432 ─ 0.806 μg/mL, 0.576 ─ 0.723 μg/mL, 0.635 ─ 0.752 μg/mL and 0.655 ─ 0.732 μg/mL for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and those for intra day precision were 0.323 ─ 0.968 μg/mL, 0.805 ─ 0.854 μg/mL, 0.078 ─ 0.844 μg/mL and 0.275 ─ 0.829 μg/mL, respectively. The intra day accuracies were 99.589% ─ 100.821%, 98.588% ─ 101.084%, 9.289% ─ 100.88%, and 98.292% ─ 101.022% for quercetin, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively, and the

  1. HPLC studies of aquatic humic compounds and complexes from the Drigg research site, Cumbria

    International Nuclear Information System (INIS)

    Smith, B.

    1992-01-01

    The work described in this report forms part of a multidisciplinary project, the broad objective of which is to study the ability of natural organic compounds present in groundwater to form mobile complexes with radionuclides. Other components of this work include the development of High Performance Liquid Chromatogaphic techniques (HPLC) to extract natural organic material from groundwater with minimal alteration, the separation of those organic fractions that complex with cations, and the development of geochemical speciation models to describe or predict metal binding. 17 Refs., 25 Figs., 4 Tabs

  2. Reverse-phase HPLC analysis of human alpha crystallin.

    Science.gov (United States)

    Swamy, M S; Abraham, E C

    1991-03-01

    A rapid and highly sensitive reverse-phase HPLC (RP-HPLC) method was used to separate crystallin subunits from human alpha crystallin. Three distinct peaks were separated; by electrophoretic and immunological analyses the first and second peaks were identified as alpha B and alpha A respectively. On the other hand, peak 3 appeared to be a modified form of alpha crystallin. The ratio of alpha A and alpha B proteins was 3:1 in 1 day old lenses which gradually changed to 2:1 in 17 year old lenses and to 1:1 in the 50 and 82 year old whole lenses and 82 year old lens cortex, with a concomitant increase in the modified alpha, suggesting that alpha A subunits are relatively more involved in aggregation. Analysis of the 82 year old lens nucleus also supported this conclusion. The RP-HPLC analysis of the HMW aggregate fraction showed substantial enrichment of the modified alpha. The alpha A and alpha B subunits independently reassociated to form polymeric alpha crystallin whereas the modified alpha reassociated to form HMW aggregates as shown by molecular sieve HPLC. Hence it appears that the HMW aggregate peak was constituted by modified alpha crystallin. Only in the peak 3 material the 280 nm absorbance was about 2-fold higher than what was expected from the actual protein content. The data suggest that the changes induced by post-translational modifications may have some role in the formation of modified alpha. The present RP-HPLC method is useful in separating these modified alpha from the unmodified alpha A and alpha B subunits.

  3. Analysis of taxines in Taxus plant material and cell cultures by hplc photodiode array and hplc-electrospray mass spectrometry

    NARCIS (Netherlands)

    Theodoridis, G.; Laskaris, G.; Rozendaal, E.L.M.; Verpoorte, R.

    2001-01-01

    A semi-purified Taxus baccata needles extract was analysed by RP-HPLC. More than 18 taxines and cinnamates were detected by photodiode array detection and LC-MS, 10 of them being positively identified. Furthermore, 10-deacetyl baccatin III (paclitaxel's main precursor) and other taxanes were also

  4. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  5. Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC); Separacion e identificacion del beta-caroteno y sus isomeros cis por cromatografia liquida de alta resolucion (HPLC)

    Energy Technology Data Exchange (ETDEWEB)

    Carrillo de Padilla, F [Universidad Central de Venezuela (UCV), Facultad de Farmacia, Catedra de Analisis de Alimentos, Caracas (Venezuela)

    1996-07-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as Mobil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproducibility, and the use of a standard of reference of a response factor for calculations.

  6. Determination of the design space of the HPLC analysis of water-soluble vitamins.

    Science.gov (United States)

    Wagdy, Hebatallah A; Hanafi, Rasha S; El-Nashar, Rasha M; Aboul-Enein, Hassan Y

    2013-06-01

    Analysis of water-soluble vitamins has been tremendously approached through the last decades. A multitude of HPLC methods have been reported with a variety of advantages/shortcomings, yet, the design space of HPLC analysis of these vitamins was not defined in any of these reports. As per the food and drug administration (FDA), implementing the quality by design approach for the analysis of commercially available mixtures is hypothesized to enhance the pharmaceutical industry via facilitating the process of analytical method development and approval. This work illustrates a multifactorial optimization of three measured plus seven calculated influential HPLC parameters on the analysis of a mixture containing seven common water-soluble vitamins (B1, B2, B6, B12, C, PABA, and PP). These three measured parameters are gradient time, temperature, and ternary eluent composition (B1/B2) and the seven calculated parameters are flow rate, column length, column internal diameter, dwell volume, extracolumn volume, %B (start), and %B (end). The design is based on 12 experiments in which, examining of the multifactorial effects of these 3 + 7 parameters on the critical resolution and selectivity, was carried out by systematical variation of all these parameters simultaneously. The 12 basic runs were based on two different gradient time each at two different temperatures, repeated at three different ternary eluent compositions (methanol or acetonitrile or a mixture of both). Multidimensional robust regions of high critical R(s) were defined and graphically verified. The optimum method was selected based on the best resolution separation in the shortest run time for a synthetic mixture, followed by application on two pharmaceutical preparations available in the market. The predicted retention times of all peaks were found to be in good match with the virtual ones. In conclusion, the presented report offers an accurate determination of the design space for critical resolution in the

  7. Previously unreported abnormalities in Wolfram Syndrome Type 2.

    Science.gov (United States)

    Akturk, Halis Kaan; Yasa, Seda

    2017-01-01

    Wolfram syndrome (WFS) is a rare autosomal recessive disease with non-autoimmune childhood onset insulin dependent diabetes and optic atrophy. WFS type 2 (WFS2) differs from WFS type 1 (WFS1) with upper intestinal ulcers, bleeding tendency and the lack ofdiabetes insipidus. Li-fespan is short due to related comorbidities. Only a few familieshave been reported with this syndrome with the CISD2 mutation. Here we report two siblings with a clinical diagnosis of WFS2, previously misdiagnosed with type 1 diabetes mellitus and diabetic retinopathy-related blindness. We report possible additional clinical and laboratory findings that have not been pre-viously reported, such as asymptomatic hypoparathyroidism, osteomalacia, growth hormone (GH) deficiency and hepatomegaly. Even though not a requirement for the diagnosis of WFS2 currently, our case series confirm hypogonadotropic hypogonadism to be also a feature of this syndrome, as reported before. © Polish Society for Pediatric Endocrinology and Diabetology.

  8. HPLC purification and re-evaluation of chemical identity of two circular bacteriocins, gassericin A and reutericin 6.

    Science.gov (United States)

    Arakawa, K; Kawai, Y; Ito, Y; Nakamura, K; Chujo, T; Nishimura, J; Kitazawa, H; Saito, T

    2010-04-01

    The study aimed for the complete purification and recharacterization of the highly hydrophobic circular bacteriocins, gassericin A and reutericin 6. Gassericin A and reutericin 6 were purified to homogeneity using previously described method and reverse-phase HPLC with an octyl column and eluents of aqueous acetonitrile and 2-propanol. Mass analysis, N-terminal sequencing and bacteriocin assay of the HPLC-purified bacteriocins showed the two bacteriocins had identical seamless circular structures with the same m/z value (5651) of [M + H](+) and both had the same specific activity. D/L-amino acid composition analysis using two distinct methods with the chiral fluorescent derivatization reagents (+)-1-(9-fluorenyl)ethyl chloroformate and O-phthalaldehyde/N-acetyl-L-cystein revealed neither gassericin A nor reutericin 6 contained D-alanine residues contrary to our previous results. Purified gassericin A and reutericin 6 are chemically identical circular molecules containing no D-alanine residues. The HPLC conditions developed in this study will facilitate advanced purification and correct characterization of other highly hydrophobic bacteriocins.

  9. [Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC)].

    Science.gov (United States)

    Carrillo de Padilla, F

    1996-06-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as movil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproductibility, and the use of a standard of reference of a response factor for calculations.

  10. Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

    Directory of Open Access Journals (Sweden)

    Andrea N. de L. Batista

    2011-06-01

    Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

  11. Development and validation of a HPLC method for standardization of herbal and commercial extracts of Myrcia uniflora

    Directory of Open Access Journals (Sweden)

    Andrea N. de L. Batista

    2011-04-01

    Full Text Available Myrcia uniflora Barb. Rodr., Myrtaceae, popularly known as "pedra-hume-caá" in Brazil, is sold as dry extracts in capsules or as tinctures for the treatment of diabetes mellitus. Previous phytochemical studies on this species described the occurrence of the flavonoids mearnsitrin and myricitrin. In the present study, the chromatographic profiles of M. uniflora leaves and commercial extracts were determined using HPLC-PAD. Myricitrin was used as an external standard in the development and validation of the HPLC method. The proposed method is simple, rapid and reliable and can be successfully applied in industry for standardization of herbs and phytomedicines commercialised in Brazil as "pedra-hume-caá".

  12. Separation and identification of beta-carotene and its cis isomers by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Carrillo de Padilla, F.

    1996-01-01

    The separation and identification by HPLC of the cis isomers of beta-carotene was studied. A 1.26 mg/ml beta-carotene solution previously isomerized with iodine as a catalyst, was eluted with 2% acetone in hexane, from a Ca(OH)2 chromatographic column in three bands. The fractions were identified by spectrophotometry and the retention times of 2.05, 2.4 and 2.8 min for the 13 cis, all-trans, and 9 cis beta-carotene isomers, determined by HPLC, with 1% acetone in hexane as Mobil phase. 22.13 mg % of all-trans beta-carotene were found in a sample of canned carrots. It is recommended the analyses of a greater number of samples, the determination of the method's sensitivity, reproducibility, and the use of a standard of reference of a response factor for calculations

  13. 77 FR 70176 - Previous Participation Certification

    Science.gov (United States)

    2012-11-23

    ... participants' previous participation in government programs and ensure that the past record is acceptable prior... information is designed to be 100 percent automated and digital submission of all data and certifications is... government programs and ensure that the past record is acceptable prior to granting approval to participate...

  14. On the Tengiz petroleum deposit previous study

    International Nuclear Information System (INIS)

    Nysangaliev, A.N.; Kuspangaliev, T.K.

    1997-01-01

    Tengiz petroleum deposit previous study is described. Some consideration about structure of productive formation, specific characteristic properties of petroleum-bearing collectors are presented. Recommendation on their detail study and using of experience on exploration and development of petroleum deposit which have analogy on most important geological and industrial parameters are given. (author)

  15. Subsequent pregnancy outcome after previous foetal death

    NARCIS (Netherlands)

    Nijkamp, J. W.; Korteweg, F. J.; Holm, J. P.; Timmer, A.; Erwich, J. J. H. M.; van Pampus, M. G.

    Objective: A history of foetal death is a risk factor for complications and foetal death in subsequent pregnancies as most previous risk factors remain present and an underlying cause of death may recur. The purpose of this study was to evaluate subsequent pregnancy outcome after foetal death and to

  16. Vergelijking van HPLC-methoden voor de bepaling van pentachloorfenol in houtmonsters

    NARCIS (Netherlands)

    Goewie; C.E.; Berkhoff; C.J.

    1986-01-01

    Een vergelijkend onderzoek is verricht naar de bruikbaarheid van verschillende detectiemethoden in combinatie met HPLC voor de analyse van pentachloorfenol in hout. In het onderzoek wordt RP-HPLC met UK en amperometrische detectie beschreven, evenals NP-HPLC met elektroneninvangdetectie. In

  17. Discovery of C5-C17 poly- and perfluoroalkyl substances in water by in-line SPE-HPLC-Orbitrap with in-source fragmentation flagging.

    Science.gov (United States)

    Liu, Yanna; Pereira, Alberto Dos Santos; Martin, Jonathan W

    2015-04-21

    The presence of unknown organofluorine compounds in environmental samples has prompted the development of nontargeted analytical methods capable of detecting new perfluoroalkyl and polyfluoroalkyl substances (PFASs). By combining high volume injection with high performance liquid chromatography (HPLC) and ultrahigh resolution Orbitrap mass spectrometry, a sensitive (0.003-0.2 ng F/mL for model mass-labeled PFASs) untargeted workflow was developed for discovery and characterization of novel PFASs in water. In the first step, up to 5 mL of water is injected to in-line solid phase extraction, chromatographed by HPLC, and detected by electrospray ionization with mass spectral acquisition in parallel modes cycling back and forth: (i) full scan with ultrahigh resolving power (RP = 120,000, mass accuracy ≤3 ppm), and (ii) in-source fragmentation flagging scans designed to yield marker fragment ions including [C2F5](-) (m/z 118.992), [C3F7](-) (m/z 168.988), [SO4H](-) (m/z 96.959), and [Cl](-) (m/z 34.9). For flagged PFASs, plausible empirical formulas were generated from accurate masses, isotopic patterns, and fragment ions. In the second step, another injection is made to collect high resolution MS/MS spectra of suspect PFAS ions, allowing further confirmation of empirical formulas while also enabling preliminary structural characterization. The method was validated by applying it to an industrial wastewater, and 36 new PFASs were discovered. Of these, 26 were confidently assigned to 3 new PFAS classes that have not previously been reported in the environment: polyfluorinated sulfates (CnFn+3Hn-2SO4(-); n = 5, 7, 9, 11, 13, and 15), chlorine substituted perfluorocarboxylates (ClCnF2nCO2(-); n = 4-11), and hydro substituted perfluorocarboxylates (HCnF2nCO2(-); n = 5-16). Application of the technique to environmental water samples is now warranted.

  18. RP-HPLC-DAD-ESI-QTOF-MS based metabolic profiling of the potential Olea europaea by-product "wood" and its comparison with leaf counterpart.

    Science.gov (United States)

    Ammar, Sonda; Contreras, Maria Del Mar; Gargouri, Boutheina; Segura-Carretero, Antonio; Bouaziz, Mohamed

    2017-05-01

    Olea europaea L. organs such as leaves, stems and roots have been associated with numerous in vivo and in vitro biological activities and used for traditional medicinal purposes. However, tree wood is an untapped resource with little information about their chemical composition. That is why, the objective of this study is to increase the knowledge about phytochemicals from 'Chemlali' olive wood by means of mass spectrometry-based analyses. Its comparison with by-products derived from leaves was also studied. Hydromethanol extracts from wood and leaves with stems of 'Chemlali' olive cultivar were analysed using reversed-phase (RP) high-performance liquid chromatography (HPLC) coupled to two detection systems: diode-array detection (DAD) and quadrupole time-of-flight (QTOF) mass spectrometry (MS) in negative ion mode. Tandem MS experiments were performed to establish the chemical structure of olive phytochemicals. A total of 85 compounds were characterised in the studied olive parts and classified as: sugars (3), organic acids (5), one phenolic aldehyde, simple phenolic acids (6), simple phenylethanoids (5), flavonoids (14), coumarins (3), caffeoyl phenylethanoid derivatives (6), iridoids (5), secoiridoids (32), and lignans (5). To our knowledge, the major part of these metabolites was not previously reported in olive tree wood, and 10 olive chemical constituents were identified for the first time in the Oleaceae family. The results presented here demonstrated the usefulness of the methodology proposed, based on RP-HPLC-DAD-ESI-QTOF-MS and MS/MS, to develop an exhaustive metabolic profiling and to recover new biologically active compounds in olive wood with pharmacologic and cosmetic potential. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  19. [Studies on fingerprinting of Flos Buddleja by RP-HPLC].

    Science.gov (United States)

    Han, Peng; Cui, Ya-jun; Guo, Hong-zhu; Guo, De-an

    2004-10-01

    To establish fingerprinting of Flos Buddleja by using RP-HPLC for the quality control. The HPLC condition was as follows: Inertsil ODS-3 C18 analytical column (4.6 mm x 250 mm, 5 microm), gredient eluation with MeCN (0.1% TFA)-H2O (0.1%TFA), flow rate 1.0 mL x min(-1), detection wavelength 254 nm. 10 commercial samples were analyzed to establish a fingerprinting. Among the obtained fingerprinting, most of the detected peaks were separated effectively. The accuracy, repeatability and stability of this method were satisfied. The RSDs of relative retention time and area of aimed peaks which existed in all samples wereless than 5%. Theresults were in accordance with the request of fingerprinting. The established fingerprinting can be used for the quality control of Flos Buddleja.

  20. HPLC-DAD determination of imidacloprid in onion

    OpenAIRE

    Mandić Aljoša; Lazić Sanja; Inđić Dušanka

    2003-01-01

    Imidacloprid is an insecticide most commonly used on vegetables, potato sugar beet, fruit, cereal, maize and rice. Imidacloprid residue has been determined in spiked onion and in onion samples. Sample preparation consisted of dichlormethane extraction of imidacloprid from onion, followed by purification of the obtained extract on a LC-Florisil disposable cartridge. The HPLC-DAD method bas been developed on reversed-phase for separation of imidacloprid with a mixture of 0.01 M phosphate buffer...

  1. Optimalizace HPLC metody pro separaci tetracyklinových antibiotik

    OpenAIRE

    Kučerová, Gabriela

    2011-01-01

    The aim of this work is to develop and to optimize HPLC method for separation of a set of four tetracycline antibiotics - tetracycline, chlortetracycline, oxytetracycline, and doxycycline. Four different reversed octadecyl-silica stationary phases in various mobile phase compositions were examined in isocratic elution. The baseline resolution of all the analytes was obtained by using two columns - Astec C18 and Atlantis C18 I. The optimized separation system consisted of Atlantis C18 I. colum...

  2. Gradient Scouting in Reversed-Phase HPLC Revisited

    Science.gov (United States)

    Alcazar, A.; Jurado, J. M.; Gonzalez, A. G.

    2011-01-01

    Gradient scouting is the best way to decide the most suitable elution mode in reversed-phase high-performance liquid chromatography (RP-HPLC). A simple rule for this decision involves the evaluation of the ratio [delta]t/t[subscript G] (where [delta]t is the difference in the retention time between the last and the first peak and t[subscript G] is…

  3. [Determination of genkwanin in flos Genkwa by HPLC].

    Science.gov (United States)

    Zhang, B; Yuan, S; Xia, K

    1996-04-01

    In this paper, the method for determining genkwanin in Flos Genkwa was established by HPLC. Detected at 332nm on a Lichrosorb 5 RP-18 column with a mobile phase of methanol-water-acetic acid (65:35:5), the content of genkwanin in Flos Genkwa was determined to be 0.16%. The recovery rate was 95.46% and RSD 1.15%.

  4. The Second SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-2)

    Science.gov (United States)

    2005-01-01

    Eight international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a variety of laboratory standards. The field samples were collected primarily from eutrophic waters, although mesotrophic waters were also sampled to create a dynamic range in chlorophyll concentration spanning approximately two orders of magnitude (0.3 25.8 mg m-3). The intercomparisons were used to establish the following: a) the uncertainties in quantitating individual pigments and higher-order variables (sums, ratios, and indices); b) an evaluation of spectrophotometric versus HPLC uncertainties in the determination of total chlorophyll a; and c) the reduction in uncertainties as a result of applying quality assurance (QA) procedures associated with extraction, separation, injection, degradation, detection, calibration, and reporting (particularly limits of detection and quantitation). In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied. The culmination of the activity was a validation of the round-robin methodology plus the development of the requirements for validating an individual HPLC method. The validation process includes the measurements required to initially demonstrate a pigment is validated, and the measurements that must be made during sample analysis to confirm a method remains validated. The so-called performance-based metrics developed here describe a set of thresholds for a variety of easily-measured parameters with a corresponding set of performance categories. The aggregate set of performance parameters and categories establish a) the overall performance capability of the method, and b) whether or not the capability is consistent with the required accuracy objectives.

  5. Previously undiagnosed hemophilia patient with intracerebral hemorrhage

    Directory of Open Access Journals (Sweden)

    Eray Atalay

    2015-09-01

    Full Text Available Intracranial bleeding in hemophilia patients is a rare but a mortal complication. Diagnosis of hemophilia in adulthood is an uncommon occurrence. In this case report an adult patient with intracranial hemorrhage is presented.

  6. HPLC/MS analysis of glucose and fluorodeoxyglucose

    Energy Technology Data Exchange (ETDEWEB)

    Bruder, P; Macasek, F; Patakyova, A; Buriova, E [Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, 84215 Bratislava (Slovakia)

    2001-05-31

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  7. HPLC/MS analysis of glucose and fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Bruder, P.; Macasek, F.; Patakyova, A.; Buriova, E.

    2001-01-01

    Objective of a new method of FDG analysis development is to replace existing tests by a more complex assay. In this work, a liquid chromatography/refractive index detector/ radiometric detector/mass spectrometric detector combination (HPLC/RID/RAD/MSD) was used for development of a complex routine technique. Optimization of HPLC/MS analysis was performed investigating the MSD analytical signal as a function of various eluent composition. Solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analyzed on the Agilent 1100 HPLC/RID/DAD/MSD system either in the flow injection (FIA) mode of analysis, and after passing the samples through Zorbax C-18 column. The most intensive signals of the ions were obtained in the acetonitrile : 0.25% ammonium formate = 80:20 solutions. This eluent would be also used for the radioactive FDG analysis on the Asahipak NH2P columns. (authors)

  8. [Studies on HPLC-FPS of the saponins from Semen Ziziphi Spinosae].

    Science.gov (United States)

    Wu, He-zhen; Chen, Jing; Liu, Yan-wen

    2006-09-01

    To establish a method of HPLC-fingerprint spectrum (HPLC-FPS) for the active part in Semen Ziziphi Spinosae (SZS) in order to control the quality of SZS from different places. The gradient elution mode was applied in chromatographic separation, and data were analysed by" Similarity Evaluation software" to compare the HPLC-FPS of SZS from different places. The conditions for HPLC analysis of SZS were established and the FPS of samples from different habitats showed some differences. All components in the spectrum were separated well and the HPLC fingerprint method is repeatable. The method can be used in quality assessment of SZS.

  9. Haemophilus influenzae type f meningitis in a previously healthy boy

    DEFF Research Database (Denmark)

    Ronit, Andreas; Berg, Ronan M G; Bruunsgaard, Helle

    2013-01-01

    Non-serotype b strains of Haemophilus influenzae are extremely rare causes of acute bacterial meningitis in immunocompetent individuals. We report a case of acute bacterial meningitis in a 14-year-old boy, who was previously healthy and had been immunised against H influenzae serotype b (Hib...

  10. Process cells dismantling of EUREX pant: previous activities

    International Nuclear Information System (INIS)

    Gili, M.

    1998-01-01

    In the '98-'99 period some process cells of the EUREX pant will be dismantled, in order to place there the liquid wastes conditioning plant 'CORA'. This report resumes the previous activities (plant rinsing campaigns and inactive Cell 014 dismantling), run in the past three years and the drawn experience [it

  11. HPLC FOR CONTROL STABILITY OF QUERCETIN INJECTABLE DOSAGE FORM

    Directory of Open Access Journals (Sweden)

    Martynov AV

    2016-12-01

    Full Text Available Introduction. Quercetin is a flavone derivatives which known like a substances with vitamin activity, high antioxidant, antimutagenic and anticarcinogenic activity and many other types of biological activity. Wide usage of quercetin prevents their polyphenolic nature structure which does not allow a high bioavailability of pure quercetin when administered orally. This is associated with a wide spectrum variety of chemical reactions for the phenolic groups: from interaction with amino acid residues in proteins to reactions with amine heterocyclic alkaloids and polysaccharides. In our days Corvitin – one from the number of quercetin based drugs with sufficiently low levels all types toxicity, allergenic and has no irritating action on intravenous administration. In the same time quercetin cannot be used in full measure because of the limited number of publications with analysis methods, especially HPLC. Determining the stability over time of concentrate quercetin solution, as well as determining the stability of the concentrate to the original autoclave sterilization conditions is a promising direction in creating new drugs. Materials and methods The objective was to research quercetin soluble formulation samples in different conditions: 1 fresh dilute concentrate (0.9% sodium chloride; 2 the original dilute concentrate, which was stored at room temperature for 14 days in light and 3 similar to the first sample dilute concentrate, which went before breeding in autoclaving at 120 0 C for 20 minutes. The objects used in the studies were industrial drug-substance quercetin (Sinkea manufactured (China, the original pharmaceutical composition as the soluble form of quercetin for injection and aerosol applications, glycerol (Sigma, Polysorbat 80 (Merk, ethanol 96 %. For the HPLC – analysis, chromatograph "Milichrom A-02" (SiChrom, Knauer (Econova, Novosibirsk, Russia was used. Results and discussion Quercetin was identified using information on its

  12. Qualitative and Quantitative Analysis of Lignan Constituents in Caulis Trachelospermi by HPLC-QTOF-MS and HPLC-UV

    Directory of Open Access Journals (Sweden)

    Xiao-Ting Liu

    2015-05-01

    Full Text Available A high-performance liquid chromatography coupled with quadrupole tandem time-of-flight mass (HPLC-QTOF-MS and ultraviolet spectrometry (HPLC-UV was established for simultaneous qualitative and quantitative analysis of the major chemical constituents in Caulis Trachelospermi, respectively. The analysis was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 5 μm using a binary gradient system of water and methanol, with ultraviolet absorption at 230 nm. Based on high-resolution ESI-MS/MS fragmentation behaviors of the reference standards, the characteristic cleavage patterns of lignano-9, 9'-lactones and lignano-8'-hydroxy-9, 9'-lactones were obtained. The results demonstrated that the characteristic fragmentation patterns are valuable for identifying and differentiating lignano-9,9'-lactones and lignano-8'-hydroxy-9,9'-lactones. As such, a total of 25 compounds in Caulis Trachelospermi were unambiguously or tentatively identified via comparisons with reference standards or literature. In addition, 14 dibenzylbutyrolatone lignans were simultaneously quantified in Caulis Trachelospermi by HPLC-UV method. The method is suitable for the qualitative and quantitative analyses of dibenzylbutyrolatone lignans in Caulis Trachelospermi.

  13. 2D-HPLC-MS phosphoproteomics analysis of lung and breast carcinomas

    International Nuclear Information System (INIS)

    Rocco, M.; Rubartelli, A.

    2009-01-01

    The project was conceived as two phases. In the first phase, we planned to validate markers, or expression patterns, previously described in the literature as being characteristic of specific tumors. In a second phase, a search for new markers associated with different tumors was to be carried on, developing new 2D-HPLC methods coupled with API-ESI mass spectrometry, with the ultimate goal of their rapid identification in biological specimens. For what concerns the first phase, the most relevant data are described in (Ceccarelli et al., 2008) and further analyzed in (Rubartelli et al., 2007). In these studies, we have compared the synthesis and intracellular accumulation levels of two oxido-reductases having also an extracellular cytokine function, the macrophage inhibitory factor (MIF) and thioredoxin (Trx)

  14. Lack of evidence from HPLC 32P-post-labelling for tamoxifen-DNA adducts in the human endometrium.

    Science.gov (United States)

    Carmichael, P L; Sardar, S; Crooks, N; Neven, P; Van Hoof, I; Ugwumadu, A; Bourne, T; Tomas, E; Hellberg, P; Hewer, A J; Phillips, D H

    1999-02-01

    Tamoxifen is associated with an increased incidence of endometrial cancer in women. It is also a potent carcinogen in rat liver and forms covalent DNA adducts in this tissue. A previous study exploring DNA adducts in human endometria, utilizing thin layer chromatography 32P-postlabelling, found no evidence for adducts in tamoxifen-treated women [Carmichael,P.L., Ugwumadu,A.H.N., Neven,P., Hewer,A.J., Poon,G.K. and Phillips,D.H. (1996) Cancer Res., 56, 1475-1479]. However, subsequent work utilizing HPLC 32P-post-labelling [Hemminki,K., Ranjaniemi,H., Lindahl,B. and Moberger,B. (1996) Cancer Res., 56, 4374-4377] suggested that very low levels could be detected. We have sought to investigate this question further by reproducing the HPLC methodology at two centres, and analysing endometrial DNA from 20 patients treated with 20 mg/day tamoxifen for between 22 and 65 months. Liver DNA isolated from tamoxifen-treated rats was used as a positive control. We found no convincing evidence for tamoxifen-derived DNA adducts in human endometrium. HPLC elution profiles of post-labelled DNA from tamoxifen-treated women were indistinguishable from those obtained with DNA from 14 untreated women and from six women taking toremifene, an analogue of tamoxifen.

  15. Books average previous decade of economic misery.

    Science.gov (United States)

    Bentley, R Alexander; Acerbi, Alberto; Ormerod, Paul; Lampos, Vasileios

    2014-01-01

    For the 20(th) century since the Depression, we find a strong correlation between a 'literary misery index' derived from English language books and a moving average of the previous decade of the annual U.S. economic misery index, which is the sum of inflation and unemployment rates. We find a peak in the goodness of fit at 11 years for the moving average. The fit between the two misery indices holds when using different techniques to measure the literary misery index, and this fit is significantly better than other possible correlations with different emotion indices. To check the robustness of the results, we also analysed books written in German language and obtained very similar correlations with the German economic misery index. The results suggest that millions of books published every year average the authors' shared economic experiences over the past decade.

  16. Books Average Previous Decade of Economic Misery

    Science.gov (United States)

    Bentley, R. Alexander; Acerbi, Alberto; Ormerod, Paul; Lampos, Vasileios

    2014-01-01

    For the 20th century since the Depression, we find a strong correlation between a ‘literary misery index’ derived from English language books and a moving average of the previous decade of the annual U.S. economic misery index, which is the sum of inflation and unemployment rates. We find a peak in the goodness of fit at 11 years for the moving average. The fit between the two misery indices holds when using different techniques to measure the literary misery index, and this fit is significantly better than other possible correlations with different emotion indices. To check the robustness of the results, we also analysed books written in German language and obtained very similar correlations with the German economic misery index. The results suggest that millions of books published every year average the authors' shared economic experiences over the past decade. PMID:24416159

  17. Comparison of a specific HPLC determination of toxic aconite alkaloids in processed Radix aconiti with a titration method of total alkaloids.

    Science.gov (United States)

    Csupor, Dezso; Borcsa, Botond; Heydel, Barbara; Hohmann, Judit; Zupkó, István; Ma, Yan; Widowitz, Ute; Bauer, Rudolf

    2011-10-01

    In traditional Chinese medicine, Aconitum (Ranunculaceae) roots are only applied after processing. Nevertheless, several cases of poisoning by improperly processed aconite roots have been reported. The aim of this study was to develop a reliable analytical method to assess the amount of toxic aconite alkaloids in commercial aconite roots, and to compare this method with the commonly used total alkaloid content determination by titration. The content of mesaconitine, aconitine, and hypaconitine in 16 commercial samples of processed aconite roots was determined by an HPLC method and the total alkaloid content by indirect titration. Five samples were selected for in vivo toxicological investigation. In most of the commercial samples, toxic alkaloids were not detectable, or only traces were found. In four samples, we could detect >0.04% toxic aconite alkaloids, the highest with a content of 0.16%. The results of HPLC analysis were compared with the results obtained by titration, and no correlation was found between the two methods. The in vivo results reassured the validity of the HPLC determination. Samples with mesaconitine, aconitine, and hypaconitine content below the HPLC detection limit still contained up to 0.2% alkaloids determined by titration. Since titration of alkaloids gives no information selectively on the aconitine-type alkaloid content and toxicity of aconite roots this method is not appropriate for safety assessment. The HPLC method developed by us provides a quick and reliable assessment of toxicity and should be considered as a purity test in pharmacopoeia monographs.

  18. Antioxidant capacity and phenolic compounds of Lonicerae macranthoides by HPLC-DAD-QTOF-MS/MS.

    Science.gov (United States)

    Hu, Xin; Chen, Lin; Shi, Shuyun; Cai, Ping; Liang, Xuejuan; Zhang, Shuihan

    2016-05-30

    Lonicerae macranthoides with strong antioxidant activity is commonly used in traditional Chinese medicine and folk tea/beverage. However, detailed information about its antioxidant activity and bioactive compounds is limited. Then at first, we comparatively evaluated total phenolic content (TPC), total flavonoid content (TFC) and antioxidant activities of water extract, petroleum ether, ethyl acetate and n-butanol fractions of L. macranthoides. Ethyl acetate fraction exhibited the highest level of TPC (207.38 mg GAE/g DW), TFC (53.06 mg RE/g DW) and the best DPPH scavenge activity and reducing power. n-Butanol fraction showed the best ABTS(+) and O2(-) scavenging activities. Interestingly, water extract, ethyl acetate and n-butanol fractions showed stronger antioxidant activities than positive control, butylated hydroxytoluene (BHT). After that, thirty-one antioxidant phenolic compounds, including twenty-two phenolic acids and nine flavonoids, were screened by DPPH-HPLC experiment and then identified using HPLC-DAD-QTOF-MS/MS. It is noted that twenty-one compounds (1, 3-4, 6-17, 19, 23, 26, 28-29, and 31), as far as was known, were discovered from L. macranthoide for the first time, and eleven of them (3-4, 10-17, and 23) were reported in Lonicera species for the first time. Results indicated that L. macranthoides could serve as promising source of rich antioxidants in foods, beverages and medicines for health promotion. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Maurya, Anupam; Srivastava, Santosh Kumar [Analytical Chemistry Division, Central Institute of Medicinal and Aromatic Plants, Lucknow (India)

    2012-03-15

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 {sup m}u{sup m}) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL{sup -1} (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 {mu}g for ursolic acid, and 0.176 and 0.587 {mu}g for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  20. Determination of ursolic acid and ursolic acid lactone in the leaves of Eucalyptus tereticornis by HPLC

    International Nuclear Information System (INIS)

    Maurya, Anupam; Srivastava, Santosh Kumar

    2012-01-01

    A simple isocratic HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and ursolic acid lactone in E. tereticornis leaves. Samples were analyzed on RP-18 (4.6 x 250 mm, 5 m u m ) column with methanol and water acidified to pH 3.5 with TFA (88:12) at 210 nm. The method was validated and applied for the simultaneous quantification of the individual triterpenes in E. tereticornis extract. The calibration curves were linear over a concentration range of 0.05-0.3 mg mL -1 (r = 0.999 and 0.998, respectively). The limits of detection and quantification were 0.190 and 0.644 μg for ursolic acid, and 0.176 and 0.587 μg for ursolic acid lactone, while the percentage recoveries were 97.32 and 96.23% for ursolic acid and ursolic acid lactone, respectively. This is the first report on the HPLC method of ursolic acid lactone with high precision and accuracy. (author)

  1. Solicitation of HPLC and HPTLC Techniques for Determination of Rutin from Polyalthia longifolia Thwaites

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Zine, Sandeep Prabhakar; Chaskar, Pratip Kashinath; Une, Hemant Devidas

    2014-01-01

    Background: Polyalthia longifolia Thwaites is an important traditional plant in India. Rutin, an active constituent has been reported to possess good amount of pharmacological as well as therapeutic potential. Objective: The aim of the present study was to find out by analytical techniques how much percentage of rutin is present in the plant leaves’ ethanolic extract by analytical techniques. Materials and Methods: Shade dried leaves of Polyalthia longifolia were subjected to cold ethanolic extraction followed by monitoring the isolated rutin high-pressure liquid chromatography (HPLC) and high performance thin layer chromatography (HPTLC) after carrying out preliminary phytochemical screening. Results: Extraction yield was found to be 13.94% w/w. Phytochemical screening of the extract showed the presence of flavonoids, steroids, diterpenoids, alkaloids, saponins, tannins and phenolic compounds and mucilage. From the Rf value, the ethanolic extract was found to be having constituent identical to rutin. By HPTLC and HPLC the amount of rutin was found to be 11.60% w/w and 4.03% w/v, respectively. Conclusion: The active constituent isolated was found to be equal to rutin. PMID:25002804

  2. Analysis of a Brazilian green propolis from Baccharis dracunculifolia by HPLC-APCI-MS and GC-MS

    Directory of Open Access Journals (Sweden)

    Roberto Chang

    Full Text Available Ethanol and dichloromethane extracts of a Brazilian green propolis from Baccharis dracunculifolia were analyzed by HPLC-APCI-MS and GC-MS, respectively. The HPLC-APCI-MS technique, at the positive mode, furnished a complete and unequivocal chemical composition of the green propolis sample. It serves as fingerprint for different propolis samples. The composition of the ethanol extract consisted mainly of cinnamic acid and derivatives, flavonoids, benzoic acid and a few benzoates, non-hydroxylated aromatics, and aliphatic acids and esters, which are normally not reported in the literature because they do not absorb UV light. The main constituents of the dichloromethane extract were prenylated compounds, alkanes and terpenoids.

  3. An Overview of Analytical Determination of Diltiazem, Cimetidine, Ranitidine, and Famotidine by UV Spectrophotometry and HPLC Technique

    Directory of Open Access Journals (Sweden)

    Nighat Shafi

    2013-01-01

    Full Text Available This review article recapitulates the analytical methods for the quantitative determinations of diltiazem and three H2 receptor antagonists (cimetidine, ranitidine, and famotidine by one of the spectroscopic technique (UV spectrophotometery and separation technique such as high-performance liquid chromatography (HPLC. The clinical and pharmaceutical analysis of these drugs requires effective analytical procedures for quality control, pharmaceutical dosage formulations, and biological fluids. An extensive survey of the literature published in various analytical and pharmaceutical chemistry-related journals has been compiled in its review. A synopsis of reported spectrophotometric and high-performance liquid chromatographic methods for individual drug is integrated. This appraisal illustrates that majority of the HPLC methods reviewed are based on the quantitative analysis of drugs in biological fluids, and they are appropriate for therapeutic drug monitoring purpose.

  4. Previous Experience a Model of Practice UNAE

    OpenAIRE

    Ormary Barberi Ruiz; María Dolores Pesántez Palacios

    2017-01-01

    The statements presented in this article represents a preliminary version of the proposed model of pre-professional practices (PPP) of the National University of Education (UNAE) of Ecuador, an urgent institutional necessity is revealed in the descriptive analyzes conducted from technical support - administrative (reports, interviews, testimonials), pedagogical foundations of UNAE (curricular directionality, transverse axes in practice, career plan, approach and diagnostic examination as subj...

  5. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-09-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetone+acrolein. Three different types of samples (rural, urban, petrol emission) were successfully analyzed

  6. Determination of carbonyl compounds in air by HPLC

    International Nuclear Information System (INIS)

    Garcia, S.; Perez, R.M.; Campos, A.; Gonzalez, D.

    1995-01-01

    A method for the determination of seven carbonyl compounds in air is presented. The procedure involve sampling of air by a Sep-Pak Cartridge impregnated with 2,4-dinitrophenylhydrazine. Elution was done with 3 mL of acetonitrile and the eluate was diluted to 5 mL. The analysis was done by HPLC with UV detection and external standard method quantification. It has been achieved relative standard deviations about 5% and detection limits of 80 ng/cartridge for formaldehyde, acetaldehyde and acetoacetonitrile. Three different types of samples (rural, urban, petrol emission) were successfully analyzed. (Author) 12 refs

  7. [Determination of 10-HDA in honeybee body by HPLC].

    Science.gov (United States)

    Fan, H; He, C; Han, H

    1999-05-01

    In the present work we found that in the honeybee body there exists an unsaturated fatty acid, trans-10-hydroxy-2-decenoic acid (10-HDA), which was known only to be present in royal jelly. We established the analytical method of 10-HDA in honeybee body by HPLC and simplified the extraction method of 10-HDA. In the optimum conditions the linear range of detection was 10-1,000 ng, the correlation coefficient was 0.9998, the recovery was 96.5%-99.2% and the detectable limit was 0.53 microgram/g.

  8. Secondary recurrent miscarriage is associated with previous male birth.

    LENUS (Irish Health Repository)

    Ooi, Poh Veh

    2012-01-31

    Secondary recurrent miscarriage (RM) is defined as three or more consecutive pregnancy losses after delivery of a viable infant. Previous reports suggest that a firstborn male child is associated with less favourable subsequent reproductive potential, possibly due to maternal immunisation against male-specific minor histocompatibility antigens. In a retrospective cohort study of 85 cases of secondary RM we aimed to determine if secondary RM was associated with (i) gender of previous child, maternal age, or duration of miscarriage history, and (ii) increased risk of pregnancy complications. Fifty-three women (62.0%; 53\\/85) gave birth to a male child prior to RM compared to 32 (38.0%; 32\\/85) who gave birth to a female child (p=0.002). The majority (91.7%; 78\\/85) had uncomplicated, term deliveries and normal birth weight neonates, with one quarter of the women previously delivered by Caesarean section. All had routine RM investigations and 19.0% (16\\/85) had an abnormal result. Fifty-seven women conceived again and 33.3% (19\\/57) miscarried, but there was no significant difference in failure rates between those with a previous male or female child (13\\/32 vs. 6\\/25, p=0.2). When patients with abnormal results were excluded, or when women with only one previous child were considered, there was still no difference in these rates. A previous male birth may be associated with an increased risk of secondary RM but numbers preclude concluding whether this increases recurrence risk. The suggested association with previous male birth provides a basis for further investigations at a molecular level.

  9. Secondary recurrent miscarriage is associated with previous male birth.

    LENUS (Irish Health Repository)

    Ooi, Poh Veh

    2011-01-01

    Secondary recurrent miscarriage (RM) is defined as three or more consecutive pregnancy losses after delivery of a viable infant. Previous reports suggest that a firstborn male child is associated with less favourable subsequent reproductive potential, possibly due to maternal immunisation against male-specific minor histocompatibility antigens. In a retrospective cohort study of 85 cases of secondary RM we aimed to determine if secondary RM was associated with (i) gender of previous child, maternal age, or duration of miscarriage history, and (ii) increased risk of pregnancy complications. Fifty-three women (62.0%; 53\\/85) gave birth to a male child prior to RM compared to 32 (38.0%; 32\\/85) who gave birth to a female child (p=0.002). The majority (91.7%; 78\\/85) had uncomplicated, term deliveries and normal birth weight neonates, with one quarter of the women previously delivered by Caesarean section. All had routine RM investigations and 19.0% (16\\/85) had an abnormal result. Fifty-seven women conceived again and 33.3% (19\\/57) miscarried, but there was no significant difference in failure rates between those with a previous male or female child (13\\/32 vs. 6\\/25, p=0.2). When patients with abnormal results were excluded, or when women with only one previous child were considered, there was still no difference in these rates. A previous male birth may be associated with an increased risk of secondary RM but numbers preclude concluding whether this increases recurrence risk. The suggested association with previous male birth provides a basis for further investigations at a molecular level.

  10. Previous Experience a Model of Practice UNAE

    Directory of Open Access Journals (Sweden)

    Ormary Barberi Ruiz

    2017-02-01

    Full Text Available The statements presented in this article represents a preliminary version of the proposed model of pre-professional practices (PPP of the National University of Education (UNAE of Ecuador, an urgent institutional necessity is revealed in the descriptive analyzes conducted from technical support - administrative (reports, interviews, testimonials, pedagogical foundations of UNAE (curricular directionality, transverse axes in practice, career plan, approach and diagnostic examination as subject nature of the pre professional practice and the demand of socio educational contexts where the practices have been emerging to resize them. By relating these elements allowed conceiving the modeling of the processes of the pre-professional practices for the development of professional skills of future teachers through four components: contextual projective, implementation (tutoring, accompaniment (teaching couple and monitoring (meetings at the beginning, during and end of practice. The initial training of teachers is inherent to teaching (academic and professional training, research and links with the community, these are fundamental pillars of Ecuadorian higher education.

  11. First characterisation of flavonoid- and diarylheptanoid-type antioxidant phenolics in Corylus maxima by HPLC-DAD-ESI-MS.

    Science.gov (United States)

    Riethmüller, Eszter; Tóth, Gergő; Alberti, Ágnes; Végh, Krisztina; Burlini, Ilaria; Könczöl, Árpád; Balogh, György Tibor; Kéry, Ágnes

    2015-03-25

    Corylus maxima Mill. (Betulaceae) leaves have been used in traditional medicine both internally and externally, nevertheless phytochemical exploration of the plant remains incomplete. In this study, the in vitro antioxidant activity and polyphenolic composition of the ethyl acetate and methanolic extracts of C. maxima leaves and bark are reported for the first time. The radical scavenging activities of the extracts were investigated by the ABTS and DPPH assays. All the extracts of C. maxima possessed notable antioxidant activity. By mean of a HPLC-DAD-ESI-TOF and a HPLC-DAD-ESI-MS/MS method, altogether twenty-two phenolics were tentatively characterised: one flavan derivative (1), seven flavonol derivatives (4, 6, 12, 13, 16, 20 and 21) and fourteen diarylheptanoids (2, 3, 5, 7-11, 14, 15, 17-19 and 22). The amount of the two main flavonoids - myricetin-3-O-rhamnoside (6) and quercetin-3-O-rhamnoside (13) - and two diarylheptanoids - oregonin (3) and hirsutenone (15) - in the extracts were determined by a validated HPLC-ESI-MS/MS method in multiple reaction monitoring (MRM) mode. Our results showed that C. maxima could be considered as a valuable source of pharmacologically important natural products that might contribute to the revaluation of the phytotherapeutical potential of the plant. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Identification of ionic chloroacetanilide-herbicide metabolites in surface water and groundwater by HPLC/MS using negative ion spray

    Science.gov (United States)

    Ferrer, I.; Thurman, E.M.; Barcelo, D.

    1997-01-01

    Solid-phase extraction (SPE) was combined with high-performance liquid chromatography/high-flow pneumatically assisted electrospray mass spectrometry (HPLC/ESP/MS) for the trace analysis of oxanilic and sulfonic acids of acetochlor, alachlor, and metolachlor. The isolation procedure separated the chloroacetanilide metabolites from the parent herbicides during the elution from C18 cartridges using ethyl acetate for parent compounds, followed by methanol for the anionic metabolites. The metabolites were separated chromatographically using reversed-phase HPLC and analyzed by negative-ion MS using electrospray ionization in selected ion mode. Quantitation limits were 0.01 ??g/L for both the oxanilic and sulfonic acids based on a 100-mL water sample. This combination of methods represents an important advance in environmental analysis of chloroacetanilide-herbicide metabolites in surface water and groundwater for two reasons. First, anionic chloroacetanilide metabolites are a major class of degradation products that are readily leached to groundwater in agricultural areas. Second, anionic metabolites, which are not able to be analyzed by conventional methods such as liquid extraction and gas chromatography/mass spectrometry, are effectively analyzed by SPE and high-flow pneumatically assisted electrospray mass spectrometry. This paper reports the first HPLC/MS identification of these metabolites in surface water and groundwater.

  13. Size Exclusion HPLC Detection of Small-Size Impurities as a Complementary Means for Quality Analysis of Extracellular Vesicles

    Directory of Open Access Journals (Sweden)

    Tao Huang

    2015-07-01

    Full Text Available For extracellular vesicle research, whether for biomarker discoveries or therapeutic applications, it is critical to have high-quality samples. Both microscopy and NanoSight Tracking Analysis (NTA for size distribution have been used to detect large vesicles. However, there is currently no well-established method that is convenient for routine quality analysis of small-size impurities in vesicle samples. In this paper we report a convenient method, called ‘size-exclusion high-performance liquid chromatography’ (SE-HPLC, alongside NTA and Microscopy analysis to guide and qualify the isolation and processing of vesicles. First, the SE-HPLC analysis was used to detect impurities of small-size proteins during the ultra-centrifugation process of vesicle isolation; it was then employed to test the changes of vesicles under different pH conditions or integrity after storage. As SE-HPLC is generally accessible in most institutions, it could be used as a routine means to assist researchers in examining the integrity and quality of extracellular vesicles along with other techniques either during isolation/preparation or for further engineering and storage.

  14. [Determination method of polysorbates in powdered soup by HPLC].

    Science.gov (United States)

    Takeda, Y; Abe, Y; Ishiwata, H; Yamada, T

    2001-04-01

    A method for qualitative and quantitative analyses of polysorbates in powdered soup by HPLC was studied. Polysorbates in samples were extracted with acetonitrile after rinsing with n-hexane to remove fats and oils. The extract was cleaned up using a Bond Elut silica gel cartridge (500 mg). The cartridge was washed with ethyl acetate and polysorbates were eluted with a small amount of acetonitrile-methanol (1:2) mixture. The eluate was treated with cobalt thiocyanate solution to form a blue complex with polysorbate. In order to determine polysorbate, the complex was subjected to HPLC with a GPC column, using a mixture of acetonitrile-water (95:5) as a mobile phase, with a detection wavelength of 620 nm. The recoveries of polysorbate 80 added to powdered soups were more than 75% and the determination limit was 0.04 mg/g. When the proposed method was applied to the determination of polysorbates in 16 commercial samples of powdered soup for instant noodles and seasoning consomme, no polysorbates were detected in any sample.

  15. Pungency Quantitation of Hot Pepper Sauces Using HPLC

    Science.gov (United States)

    Betts, Thomas A.

    1999-02-01

    A class of compounds known as capsaicinoids are responsible for the "heat" of hot peppers. To determine the pungency of a particular pepper or pepper product, one may quantify the capsaicinoids and relate those concentrations to the perceived heat. The format of the laboratory described here allows students to collectively develop an HPLC method for the quantitation of the two predominant capsaicinoids (capsaicin and dihydrocapsaicin) in hot-pepper products. Each small group of students investigated one of the following aspects of the method: detector wavelength, mobile-phase composition, extraction of capsaicinoids, calibration, and quantitation. The format of the lab forced students to communicate and cooperate to develop this method. The resulting HPLC method involves extraction with acetonitrile followed by solid-phase extraction clean-up, an isocratic 80:20 methanol-water mobile phase, a 4.6 mm by 25 cm C-18 column, and UV absorbance detection at 284 nm. The method developed by the students was then applied to the quantitation of capsaicinoids in a variety of hot pepper sauces. Editor's Note on Hazards in our April 2000 issue addresses the above.

  16. Analysis of the radiochemical purity of 18F-FDG by HPLC

    International Nuclear Information System (INIS)

    Chen Liguang; Tang Anwu; He Shanzhen; Chen Yulong

    2001-01-01

    The radiochemical purity (RCP) of 18 F-FDG is analyzed by HPLC. Eighty-five percent acetonitrile is used as the eluting solution. Carbon hydrate column is used as separation column. The t R of 18 F - is 6.50 min and 18 F-FDG is 9.00 min. HPLC take less time and has higher sensitivity than TLC for the same sample at the same time. So HPLC excels TLC in analyzing RCP of 18 F-FDG

  17. Multi-Analyte Separation Methods for HPLC Determination of the Active Ingredients of Pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Virtics, I.; Korsós, I.; Homoki, E.; Lantos, J. [Plant Protection and Soil Conservation Service of Szabolcs-Szatmár-Bereg County, Nyíregyháza (Hungary)

    2009-07-15

    The practical quality control of selected pesticides, such as carbamates, organophosphorous compounds, phthalimides, pyrethroids, with HPLC is described. Detailed descriptions are given of materials and methods used, including sample preparation and HPLC operating conditions. The relationship between pH value of the HPLC eluent and the logP{sub ow} is discussed, illustrated by chromatograms, graphics and tables. The results are also compared with those elaborated by. E. Dudar and presented above. (author)

  18. Analysis of in vivo absorption of didanosine tablets in male adult dogs by HPLC

    Directory of Open Access Journals (Sweden)

    Patrícia Severino

    2012-02-01

    Full Text Available Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV. An automated system using on-line solid extraction and High Performance Liquid Chromatography (HPLC with ultraviolet (UV detection was developed and validated for pharmacokinetic analysis of didanosine in dog plasma. Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma. Extraction was carried out on C18 cartridges, with high extraction yield as stationary phase, whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer, acetonitrile (KH2PO4: acetonitrile: 96:4, v/v and 0.5% (w/v of heptane sulphonic acid. The pH was adjusted to 6.5 with triethylamine. All samples and standard solutions were chromatographed at 28 °C. For an isocratic run, the flux was 1.0 mL/min, detection was at 250 nm and injected volume was 20 μL. The method was selective and linear for concentrations between 50 and 5000 ng/mL. Drug stability data ranged from 96% to 98%, and limit of quantification was 25 ng/mL. Extraction yield was up to 95%. Drug stability in dog plasma was kept frozen at −20 °C for one month after three freeze–thaw cycles, and for 24 h after processing in the auto sampler. Assay was successfully applied to measure didanosine concentrations in plasma dogs. Keywords: Didanosine, On-line solid phase extraction, HPLC, Male dogs

  19. The Fourth SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-4)

    Science.gov (United States)

    Hooker, Stanford B.; Thomas, Crystal S.; van Heukelem, Laurie; Schlueter, louise; Russ, Mary E.; Ras, Josephine; Claustre, Herve; Clementson, Lesley; Canuti, Elisabetta; Berthon, Jean-Francois; hide

    2010-01-01

    Ten international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a mixed pigment sample. Although prior Sea-viewing Wide Field-of-view Sensor (SeaWiFS) High Performance Liquid Chromatography (HPLC) Round-Robin Experiment (SeaHARRE) activities conducted in open-ocean waters covered a wide dynamic range in productivity, and some of the samples were collected in the coastal zone, none of the activities involved exclusively coastal samples. Consequently, SeaHARRE-4 was organized and executed as a strictly coastal activity and the field samples were collected from primarily eutrophic waters within the coastal zone of Denmark. The more restrictive perspective limited the dynamic range in chlorophyll concentration to approximately one and a half orders of magnitude (previous activities covered more than two orders of magnitude). The method intercomparisons were used for the following objectives: a) estimate the uncertainties in quantitating individual pigments and higher-order variables formed from sums and ratios; b) confirm if the chlorophyll a accuracy requirements for ocean color validation activities (approximately 25%, although 15% would allow for algorithm refinement) can be met in coastal waters; c) establish the reduction in uncertainties as a result of applying QA procedures; d) show the importance of establishing a properly defined referencing system in the computation of uncertainties; e) quantify the analytical benefits of performance metrics, and f) demonstrate the utility of a laboratory mix in understanding method performance. In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied.

  20. Development and Application of Multidimensional HPLC Mapping Method for O-linked Oligosaccharides

    Directory of Open Access Journals (Sweden)

    Koichi Kato

    2011-12-01

    Full Text Available Glycosylation improves the solubility and stability of proteins, contributes to the structural integrity of protein functional sites, and mediates biomolecular recognition events involved in cell-cell communications and viral infections. The first step toward understanding the molecular mechanisms underlying these carbohydrate functionalities is a detailed characterization of glycan structures. Recently developed glycomic approaches have enabled comprehensive analyses of N-glycosylation profiles in a quantitative manner. However, there are only a few reports describing detailed O-glycosylation profiles primarily because of the lack of a widespread standard method to identify O-glycan structures. Here, we developed an HPLC mapping method for detailed identification of O-glycans including neutral, sialylated, and sulfated oligosaccharides. Furthermore, using this method, we were able to quantitatively identify isomeric products from an in vitro reaction catalyzed by N-acetylglucosamine-6O-sulfotransferases and obtain O-glycosylation profiles of serum IgA as a model glycoprotein.

  1. Backflush HPLC for the isolation of polycyclic aromatic compounds - a comparative study

    Energy Technology Data Exchange (ETDEWEB)

    Oestman, C.E.; Colmsjoe, A.L.

    1987-12-01

    Semipreparative HPLC utilizing a polar bonded phase was applied to the isolation of polycyclic aromatic compounds (PAC) from complex samples using a backflush technique. Aminopropyl- and cyanopropyl-modified silica was tested. Aminopropyl-modified silica was found to be superior in achieving rapid, selective and non discriminating isolation of PAC. This was compared with the most commonly used isolation methods, dimethylsulfoxide (DMSO), dimethylformamide (DMF) and nitromethane liquid-liquid extractions, and silica and SephadexLH-20 open column chromatography. Strong discrimination of alkylated PAC and polycyclic aromatic nitrogen heterocyclics (PANH) was found for the liquid-liquid extractions and the LH-20 column chromatography. These comparisons were made using both standard compounds and a sample of used crank-case oil, indicating the necessity of using a real sample for evaluation of extraction methods. Recoveries of 42 PACs are reported.

  2. Determination of oxidation products in radiolysis of halophenols with pulse radiolysis, hplc, and ion chromatography

    International Nuclear Information System (INIS)

    Ye, M.; Schuler, R.H.

    1990-01-01

    This paper reports on hydroxyl radicals that react with halogen substituted phenols by several different ways. One is addition of OH radicals to the aromatic ring, which is followed by elimination of hydrogen halide, H 2 O or H - . The positions of OH radicals attack are dependent on the nature of the halogen which affects the electronic distribution in the ring. The oxidation of fluorophenols, chlorophenols and bromophenols with hydroxyl radicals in N 2 O saturated solution has been investigated with pulse radiolysis and γ-irradiation experiments. The intermediates of the reactions were studied by pulse radiolysis. The products created in the γ-irradiation of aqueous solutions of halophenols were analyzed by ion chromatography and high performance liquid chromatography (HPLC). With the combination of time-resolved and steady-state experiments a complete and detailed description of radiolytic oxidation of halophenols by hydroxyl radicals was obtained

  3. Carboxyterfenadine antacid interaction monitoring by UV spectrophotometry and RP-HPLC techniques

    Directory of Open Access Journals (Sweden)

    Hina Shehnaz

    2014-11-01

    Full Text Available Carboxyterfenadine, a primary metabolite of terfenadine, a second generation antihistaminic compound was introduced in therapy as a successor of terfenadine due to its cardiac arrhythmia. There are number of drug interactions of fexofenadine with erythromycin, ketoconazole and alike reported in the literature. In this paper, fexofenadine antacid interaction has been studied in presence of sodium bicarbonate, megaldrate, calcium carbonate, magnesium carbonate, aluminum hydroxide, magnesium hydroxide, magnesium trisilicate, simethicone (dimethylpolysiloxane and calcium hydroxide by UV–Vis spectrophotometer and high performance liquid chromatography (HPLC. These in vitro fexofenadine–antacid interactions were carried out in simulated gastric and intestinal juices and in buffer of pH 7.4 (simulating blood pH on BP 2005 dissolution apparatus. The results show non-concordant availability of fexofenadine envisaged due to formation of unstable charge transfer complexes.

  4. SPE-HPLC purification of endocrine disrupting compounds from human serum for assessment of xenoestrogenic activity

    DEFF Research Database (Denmark)

    Hjelmborg, P.S.; Ghisari, Mandana; Bonefeld-Jørgensen, Eva

    2006-01-01

    Assessment of xenoestrogenic activity in human serum samples requires the removal of endogenous sex hormones to assure that the activity measured originates from xenobiotic compounds only. Serum samples representing high, medium and lower accumulation of persistent organic pollutants (POPs) were...... measured by ERE-CALUX was validated and considered to be a valuable tool to assess the combined ER effect of lipophilic serum POPs where additive/synergistic and agonistic/antagonistic effects are integrated giving an overall estimate of exposure and bioactivity....... for the study. MVLN cells, stably transfected with an estrogen receptor (ER) luciferase reporter vector (ERE-CALUX), were exposed to the reconstituted SPE-HPLC extracts for determination of the integrated estrogenic activity. The effects of PCBs were analyzed by direct in vitro exposure of PCBs (138, 153...

  5. Determination of cadmium and lead species and phytochelatins in pea (Pisum sativum) by HPLC-ICPMS and HPLC-ESIMSn

    International Nuclear Information System (INIS)

    Baralkiewicz, D.; Magorzata, K.; Piechalak, A.; Tomaszewska, B.

    2009-01-01

    Full text: Trace elements play an important role in the functioning of life on our planet. Some of them can be highly toxic, whereas others can be essential. These effects are very often related to particular form in which the element is present. Often these different chemical forms of a particular element or its compounds are referred to as 'species'. Cadmium and lead are widespread heavy metal pollutants released into the environment by human activities. The presence of Pb 2+ and Cd 2+ in the environment leads to a numerous disturbances in many metabolic processes in plants. Inhibition of growth is a major symptom. Hyphenated techniques, such as HPLC-ICPMS and HPLC-ESIMSn seem to be the best analytical instruments to study metal speciation in plants. In our study, we used hyphenated techniques to identify compounds engaged in Cd and Pb metabolism and to perform analysis of metal complexes induced in Pisum sativum exposed to cadmium and lead. These identified compounds might be valuable source of information to study metal accumulation mechanism for bioremediation processes. (author)

  6. Determination of some psychotropic drugs in serum and saliva samples by HPLC-DAD and HPLC MS.

    Science.gov (United States)

    Petruczynik, A; Wróblewski, K; Szultka-Młyńska, M; Buszewski, B; Karakuła-Juchnowicz, H; Gajewski, J; Morylowska-Topolska, J; Waksmundzka-Hajnos, M

    2016-08-05

    A simple, rapid and sensitive HPLC-DAD method has been developed and validated for the simultaneous determination of seven psychotropic drugs (risperidone, citalopram, clozapine,quetiapine, levomepromazine, perazine and aripiprazole) in human serum or saliva samples. The chromatographic analyses were performed on a XSELECT CSH Phenyl-Hexyl column with a mobile phase containing methanol, acetate buffer at pH 3.5 and 0.025mL(-1) diethylamine. The influence of concentration of methanol in injection samples and injection volume on peak symmetry and system efficiency was examined.The full separation of all investigated drugs, good peaks' symmetry and simultaneously high systems efficiency were obtained in applied chromatographic system. The method is suitable for the analysis of investigated drugs in human plasma or saliva for psychiatric patients for control of pharmacotherapy, particularly in combination therapy. HPLC-MS was applied for verification of the presence of drugs and their metabolites in serum and saliva samples from patients. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Determination of anthocyanins from camu-camu (Myrciaria dubia) by HPLC-PDA, HPLC-MS, and NMR.

    Science.gov (United States)

    Zanatta, Cinthia Fernanda; Cuevas, Elyana; Bobbio, Florinda O; Winterhalter, Peter; Mercadante, Adriana Z

    2005-11-30

    Camu-camu [Myrciaria dubia (HBK) McVaugh] is a small fruit native to the Amazonian rain forest. Its anthocyanin profile has now been investigated for the first time. Fruits from two different regions of the São Paulo state, Brazil, were analyzed. The major anthocyanins were isolated by high-speed countercurrent chromatography. HPLC-PDA, HPLC-MS/MS, and 1H NMR were used to confirm the identity of the main anthocyanins of camu-camu. Cyanidin-3-glucoside was identified as the major pigment in the fruits from both regions, representing 89.5% in the fruits produced in Iguape and 88.0% in those from Mirandópolis, followed by the delphinidin-3-glucoside, ranging between 4.2 and 5.1%, respectively. Higher total anthocyanin contents were detected in the fruits from Iguape (54.0 +/- 25.9 mg/100 g) compared to those from Mirandópolis (30.3 +/- 6.8 mg/100 g), most likely because of the lower temperatures in the Iguape region.

  8. Squamous cell carcinoma arising in previously burned or irradiated skin

    International Nuclear Information System (INIS)

    Edwards, M.J.; Hirsch, R.M.; Broadwater, J.R.; Netscher, D.T.; Ames, F.C.

    1989-01-01

    Squamous cell carcinoma (SCC) arising in previously burned or irradiated skin was reviewed in 66 patients treated between 1944 and 1986. Healing of the initial injury was complicated in 70% of patients. Mean interval from initial injury to diagnosis of SCC was 37 years. The overwhelming majority of patients presented with a chronic intractable ulcer in previously injured skin. The regional relapse rate after surgical excision was very high, 58% of all patients. Predominant patterns of recurrence were in local skin and regional lymph nodes (93% of recurrences). Survival rates at 5, 10, and 20 years were 52%, 34%, and 23%, respectively. Five-year survival rates in previously burned and irradiated patients were not significantly different (53% and 50%, respectively). This review, one of the largest reported series, better defines SCC arising in previously burned or irradiated skin as a locally aggressive disease that is distinct from SCC arising in sunlight-damaged skin. An increased awareness of the significance of chronic ulceration in scar tissue may allow earlier diagnosis. Regional disease control and survival depend on surgical resection of all known disease and may require radical lymph node dissection or amputation

  9. Heterozygote Hemoglobin G-Coushatta as the Cause of a Falsely Decreased Hemoglobin A1C in an Ion-Exchange HPLC Method

    Directory of Open Access Journals (Sweden)

    Kurtoğlu Ayşegül Uğur

    2017-09-01

    Full Text Available Glycated hemoglobin (HbA1c is used for the assessment of glycemic control in patients with diabetes. The presence of genetic variants of hemoglobin can profoundly affect the accuracy of HbA1c measurement. Here, we report two cases of Hemoglobin G-Coushatta (HBB:c.68A>C variant that interferes in the measurement of HbA1c by a cation-exchange HPLC (CE-HPLC method. HbA1c was measured by a CE-HPLC method in a Tosoh HLC-723 G7 instrument. The HbA1c levels were 2.9% and 4%. These results alerted us to a possible presence of hemoglobinopathy. In the hemoglobin variant analysis, HbA2 levels were detected as 78.3% and 40.7% by HPLC using the short program for the Biorad Variant II. HbA1c levels were measured by an immunoturbidimetric assay in a Siemens Dimension instrument. HbA1c levels were reported as 5.5% and 5.3%. DNA mutation analysis was performed to detect the abnormal hemoglobin variant. Presence of Hemoglobin G-Coushatta variant was detected in the patients. The Hb G-Coushatta variants have an impact on the determination of glycated hemoglobin levels using CEHPLC resulting in a false low value. Therefore, it is necessary to use another measurement method.

  10. HPLC-MS technique for radiopharmaceuticals research and control

    Energy Technology Data Exchange (ETDEWEB)

    Macasek, F; Bruder, P [Department of Nuclear Chemistry, Faculty of Natural Sciences, Comenius University, Bratislava (Slovakia); Buriova, E [Cyclotron Centre of the Slovak Republic, Slovak Office of Standards, Metrology and Testing, Bratislava (Slovakia)

    2002-03-01

    A liquid chromatography/refractive index detector/radiometric detector/ mass spectrometric detector combination (Agilent 1100 HPLC/RAD/DAD/RID/MSD system) is used as a complex technique for quality assessment of radiopharmaceuticals such as 2-deoxy-2-[{sup 18}F]fluoro-D-glucose (FDG). Optimisation of HPLC/MS analysis was performed investigating the electrospray ionisation (ESI) analytical signal of the mass spectrometer as a function of solvent composition. The anion-exchange eluents applied as specified by the pharmacopoeia are not suitable for ESI detection due to high ion concentrations. Therefore, solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analysed by flow injection analysis (FIA) and chromatographically. The best analytical response was obtained with acetonitrile : 0.25% ammonium formate = 80:20 solutions. The most intense MSD signals of FDG in ammonium formate were obtained for the following complex ions: (i) positive ions: fdg.NH{sub 4}{sup +}, fdg.Na{sup +} and (fdg{sub 2}-CH{sub 3}O).Na{sup +} (m/z = 200, 205 and 344); (ii) negative ions: fdg.Cl{sup -} and fdg.HCOO{sup -} (m/z= 217 and 227). The HPLC-MS analysis with Zorbax C-18 and Asahipak-NH2P50 columns gave evidence of admixtures and radiolytic formation of deoxyglucose, deoxychloro-glucose, erythrose, erythritol, gluconic acid, lactose, raffinose, saccharic acid, sorbitol/[{sup 19}F]FDG, sorbitol/[{sup 19}F]FDG, xylitol, and other compounds. However, radiometric analysis of expired samples of [{sup 18}F]FDG gave evidence of a very high radiation stability of its water-ethanol solutions at the point of output of radioactive products. Remarkable is the exceedingly high complexity of the mass spectra of FDG as compared to glucose. Therefore, further research concerns the influence of sodium chloride, linearity of signal response, impurities (mannitol, mannose etc.) interference, and

  11. HPLC-MS technique for radiopharmaceuticals research and control

    International Nuclear Information System (INIS)

    Macasek, F.; Bruder, P.; Buriova, E.

    2002-01-01

    A liquid chromatography/refractive index detector/radiometric detector/ mass spectrometric detector combination (Agilent 1100 HPLC/RAD/DAD/RID/MSD system) is used as a complex technique for quality assessment of radiopharmaceuticals such as 2-deoxy-2-[ 18 F]fluoro-D-glucose (FDG). Optimisation of HPLC/MS analysis was performed investigating the electrospray ionisation (ESI) analytical signal of the mass spectrometer as a function of solvent composition. The anion-exchange eluents applied as specified by the pharmacopoeia are not suitable for ESI detection due to high ion concentrations. Therefore, solutions of glucose in methanol/water and acetonitrile/water solutions of various semi-volatile electrolytes (ammonium chloride, formic acid, ammonium formate) were analysed by flow injection analysis (FIA) and chromatographically. The best analytical response was obtained with acetonitrile : 0.25% ammonium formate = 80:20 solutions. The most intense MSD signals of FDG in ammonium formate were obtained for the following complex ions: (i) positive ions: fdg.NH 4 + , fdg.Na + and (fdg 2 -CH 3 O).Na + (m/z = 200, 205 and 344); (ii) negative ions: fdg.Cl - and fdg.HCOO - (m/z= 217 and 227). The HPLC-MS analysis with Zorbax C-18 and Asahipak-NH2P50 columns gave evidence of admixtures and radiolytic formation of deoxyglucose, deoxychloro-glucose, erythrose, erythritol, gluconic acid, lactose, raffinose, saccharic acid, sorbitol/[ 19 F]FDG, sorbitol/[ 19 F]FDG, xylitol, and other compounds. However, radiometric analysis of expired samples of [ 18 F]FDG gave evidence of a very high radiation stability of its water-ethanol solutions at the point of output of radioactive products. Remarkable is the exceedingly high complexity of the mass spectra of FDG as compared to glucose. Therefore, further research concerns the influence of sodium chloride, linearity of signal response, impurities (mannitol, mannose etc.) interference, and robustness of the MS analysis, with special attention

  12. Microwave-assisted extraction of herbacetin diglucoside from flax (Linum usitatissimum L.) seed cakes and its quantification using an RP-HPLC-UV system.

    Science.gov (United States)

    Fliniaux, Ophélie; Corbin, Cyrielle; Ramsay, Aina; Renouard, Sullivan; Beejmohun, Vickram; Doussot, Joël; Falguières, Annie; Ferroud, Clotilde; Lamblin, Frédéric; Lainé, Eric; Roscher, Albrecht; Grand, Eric; Mesnard, François; Hano, Christophe

    2014-03-10

    Flax (Linum usitatissimum L.) seeds are widely used for oil extraction and the cold-pressed flaxseed (or linseed) cakes obtained during this process constitute a valuable by-product. The flavonol herbacetin diglucoside (HDG) has been previously reported as a constituent of the flaxseed lignan macromolecule linked through ester bonds to the linker molecule hydroxymethylglutaric acid. In this context, the development and validation of a new approach using microwave-assisted extraction (MAE) of HDG from flaxseed cakes followed by quantification with a reverse-phase HPLC system with UV detection was purposed. The experimental parameters affecting the HDG extraction yield, such as microwave power, extraction time and sodium hydroxide concentration, from the lignan macromolecule were optimized. A maximum HDG concentration of 5.76 mg/g DW in flaxseed cakes was measured following an irradiation time of 6 min, for a microwave power of 150 W using a direct extraction in 0.1 M NaOH in 70% (v/v) aqueous methanol. The optimized method was proven to be rapid and reliable in terms of precision, repeatability, stability and accuracy for the extraction of HDG. Comparison with a conventional extraction method demonstrated that MAE is more effective and less time-consuming.

  13. Characterization and quantification of flavonoids and hydroxycinnamic acids in curly kale (Brassica oleracea L. Convar. acephala Var. sabellica) by HPLC-DAD-ESI-MSn.

    Science.gov (United States)

    Olsen, Helle; Aaby, Kjersti; Borge, Grethe Iren A

    2009-04-08

    Kale is a leafy green vegetable belonging to the Brassicaceae family, a group of vegetables including cabbage, broccoli, cauliflower, and Brussels sprouts, with a high content of health-promoting phytochemicals. The flavonoids and hydroxycinammic acids of curly kale ( Brassica oleracea L. ssp. oleracea convar. acephala (DC.) Alef. var. sabellica L.), a variety of kale, were characterized and identified primarily through HPLC-DAD-ESI-MS(n) analysis. Thirty-two phenolic compounds including glycosides of quercetin and kaempferol and derivatives of p-coumaric, ferulic, sinapic, and caffeic acid were tentatively identified, providing a more complete identification of phenolic compounds in curly kale than previously reported. Moreover, three hydroxycinnamic acids and one flavonoid with an unusual high grade of glycosylation, quercetin-3-disinapoyl-triglucoside-7-diglucoside, have been tentatively identified for the first time. The influence of different extraction conditions (extraction method, solvent type, solvent/solid ratio, and duration of extraction) was investigated. The total flavonol and hydroxycinnamic acid contents in curly kale determined as rutin equivalents (RE) were 646 and 204 mg of RE/100 g of fresh weight (fw), respectively. The contents of individual flavonoids ranged from 2 to 159 mg of RE/100 g of fw, with main compounds kaempferol-3-sinapoyl-diglucoside-7-diglucoside (18.7%) and quercetin-3-sinapoyl-diglucoside-7-diglucoside (16.5%). After acidic hydrolysis, two flavonol aglycones were identified in curly kale, quercetin and kaempferol, with total contents of 44 and 58 mg/100 g of fw, respectively.

  14. HPLC-DAD DETERMINATION OF BERBERINE, CHELERYTHRINE AND SANGUINARINE IN THE MEXICAN PRICKLY POPPY (Argemone mexicana L. PAPAVERACEAE, A MEDICINAL PLANT

    Directory of Open Access Journals (Sweden)

    Jorge F. Xool-Tamayo

    Full Text Available A sensitive, simple, rapid and reliable HPLC-DAD method for the analysis of the benzylisoquinoline alkaloids (BIA's content in Argemone mexicana (Papaveraceae is presented. This method allows the simultaneous separation and quantitation of berberine (Bn, chelerythrine (C and sanguinarine (S in extracts from A. mexicana tissues, reducing time of analysis in comparison to previous reports. Alkaloids were separated on a C18 Hypersil Gold column using an acetonitrile gradient (20 to 70% in 1% acetic acid in water. Alkaloids were identified based on retention times and UV spectra and quantified at 254 nm. Linearity between 0.5-20 µg mL-1 was observed for Bn, C and S, with limits of detection (LOD and quantitation (LOQ of 0.11 and 0.33 for Bn, 0.10 and 0.30 for C and 0.05 and 0.15 for S, respectively. Maximal intra- and inter-day variation values were < 0.49% in all cases, with alkaloids' recoveries higher than 95%. System suitability tests (SST, including resolution (Rs, retention factor (K', selectivity (α, tailing factor and number of theoretical plates were performed according to the United States Pharmacopeia (USP, fulfilling recommended values. The method proved to be efficient and reproducible when analyzing different tissues of field-collected A. mexicana plants.

  15. HPLC Determination of Polyphenols from Calendula officinalis L. Flowers

    Directory of Open Access Journals (Sweden)

    Frum Adina

    2017-12-01

    Full Text Available Romanian spontaneous flora provides a lot of resources for the determination of different chemical compounds. This study uses flower samples from Calendula officinalis L. extracted through maceration. The chemical compounds determined were: (+-catechin, caffeic acid, chlorogenic acid, cinnamic acid, ferulic acid, gallic acid, rutin, resveratrol and quercetin. They were analyzed by using an optimized HPLC method. (+-Catechin, caffeic acid, chlorogenic acid and quercetin could not be identified in the analyzed samples. The greatest amount of phenolic compound found was rutin and the smallest quantity was determined for ferulic acid. The quantified compounds have proven to have benefits regarding human health, thus they can be used as functional compounds and can be included in food products and food supplements.

  16. Quantitative analysis of PMR-15 polyimide resin by HPLC

    Science.gov (United States)

    Roberts, Gary D.; Lauver, Richard W.

    1987-01-01

    The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

  17. HPLC identification of isoniazid residues in bovine milk

    Directory of Open Access Journals (Sweden)

    Leite R.M.H.

    2000-01-01

    Full Text Available The high pressure liquid chromatography (HPLC was used for the identification of isoniazid (isonicotinic acid hydrazide in the milk of cattle treated with a dose of 25 mg/kg/day in alternated days. The effect of milk pasteurization on the isoniazid residue concentration was also studied. The drug excretion presented a cyclic variation, with higher levels in the first day after administration (aa, a mean of 1104.48µg/l, and a decrease two days aa, with a mean of 104.12µg/l. Four days after the last administration of the drug it was not possible to identify residues of isoniazid in the milk of treated animals. Body weight and milk yield influenced the amount of the excreted drug, and pasteurization decreased (mean 47.07% the concentration of isoniazid residue in milk.

  18. HPLC method validation for modernization of the tetracycline hydrochloride capsule USP monograph

    Directory of Open Access Journals (Sweden)

    Emad M. Hussien

    2014-12-01

    Full Text Available This paper is a continuation to our previous work aiming at development and validation of a reversed-phase HPLC for modernization of tetracycline-related USP monographs and the USP general chapter . Previous results showed that the method is accurate and precise for the assay of tetracycline hydrochloride and the limit of 4-epianhydrotetracycline impurity in the drug substance and oral suspension monographs. The aim of the current paper is to examine the feasibility of the method for modernization of USP tetracycline hydrochloride capsule monograph. Specificity, linearity, accuracy and precision were examined for tetracycline hydrochloride assay and 4-epianhydrotetracycline limit. The method was linear in the concentration range from 80% to 160% (r>0.9998 of the assay concentration (0.1 mg/mL for tetracycline hydrochloride and from 50% to 150% (r>0.997 of the acceptance criteria specified in tetracycline hydrochloride capsule monograph for 4-epianhydrotetracycline (NMT 3.0%. The recovery at three concentration levels for tetracycline hydrochloride assay was between 99% and 101% and the RSD from six preparations at the concentration 0.1 mg/mL is less than 0.6%. The recovery for 4-epianhydrotetracycline limit procedure over the concentration range from 50% to 150% is between 96% and 102% with RSD less than 5%. The results met the specified acceptance criteria.

  19. Simultaneous quantification of flavonoids and triterpenoids in licorice using HPLC.

    Science.gov (United States)

    Wang, Yuan-Chuen; Yang, Yi-Shan

    2007-05-01

    Numerous bioactive compounds are present in licorice (Glycyrrhizae Radix), including flavonoids and triterpenoids. In this study, a reversed-phase high-performance liquid chromatography (HPLC) method for simultaneous quantification of three flavonoids (liquiritin, liquiritigenin and isoliquiritigenin) and four triterpenoids (glycyrrhizin, 18alpha-glycyrrhetinic acid, 18beta-glycyrrhetinic acid and 18beta-glycyrrhetinic acid methyl ester) from licorice was developed, and further, to quantify these 7 compounds from 20 different licorice samples. Specifically, the reverse-phase HPLC was performed with a gradient mobile phase composed of 25 mM phosphate buffer (pH 2.5)-acetonitrile featuring gradient elution steps as follows: 0 min, 100:0; 10 min, 80:20; 50 min, 70:30; 73 min, 50:50; 110 min, 50:50; 125 min, 20:80; 140 min, 20:80, and peaks were detected at 254 nm. By using our technique, a rather good specificity was obtained regarding to the separation of these seven compounds. The regression coefficient for the linear equations for the seven compounds lay between 0.9978 and 0.9992. The limits of detection and quantification lay in the range of 0.044-0.084 and 0.13-0.25 microg/ml, respectively. The relative recovery rates for the seven compounds lay between 96.63+/-2.43 and 103.55+/-2.77%. Coefficient variation for intra-day and inter-day precisions lay in the range of 0.20-1.84 and 0.28-1.86%, respectively. Based upon our validation results, this analytical technique is a convenient method to simultaneous quantify numerous bioactive compounds derived from licorice, featuring good quantification parameters, accuracy and precision.

  20. An improved HPLC method for determination of colocynthin in colocynth

    Directory of Open Access Journals (Sweden)

    M. Shekarchi

    2015-10-01

    Full Text Available Background and objectives: Colocynthin is the major active secondary metabolite of colocynth, Citrullus colocynthis (L. Schrad, which has been used in traditional and ethno medicine of many countries.  It could be considered as an active marker for quality control of colocynth and its herbal products. Analysis and standardization of colocynth and its herbal preparations are a critical issue for their safe applications in phytotherapy and traditional medicine. In the present work, a simple and efficient sample preparation was developed and optimized through combination of matrix solid phase dispersion and ultrasonic assisted extraction. In addition, analytical reversed-phase HPLC method was optimized for analyzing the concentration of colocynthin in colocynth pulp. Methods: Powdered colocynth pulp was grinded with diatomaceous earth to obtain a homogenous mixture. The blend was mixed with methanol and extracted by sonication, followed by centrifugation and filtration. The analytical chromatographic separation was carried out using Luna C18 in isocratic elution with methanol: isopropanol: water: triflouroacetic acid (30:10:60:0.1 v/v. The method was validated as well.  Results: The validation parameters were determines as follows, linear range (r2 = 0.999, 75-500 μg/mL, precision (intra-day < 2.7%, inter-day = 4.4% and accuracy measured via determination of recovery (90-107%. The limit of detection and quantization were calculated 8.5 and 25.7 μg/mL, respectively. Conclusion: Regarding the relatively high content of colocynthin in colocynth pulp, the validated HPLC method could be applied for quality control of colocynth pulp used in Traditional Persian Medicine.

  1. Analysis of brominated and phosphate-based flame retardants in polymer samples by HPLC-UV/MS and online-GPC-HPLC-UV

    Energy Technology Data Exchange (ETDEWEB)

    Schlummer, M.; Brandl, F. [Fraunhofer-Institut fuer Verfahrenstechnik und Verpackung (IVV), Freising (Germany); Maeurer, A.

    2004-09-15

    Here we present two analytical approaches for the identification and quantification of brominated and phosphate-based flame retardants. The first is an HPLC-UV/MS approach, which allows the separation and unequivocal identification and quantification of at least 15 different technical flame retardants. The second approach was set-up as a screening tool, consisting of a GPC separation coupled to an HPLC-UV device.

  2. Comparative HPLC/ESI-MS and HPLC/DAD study of different populations of cultivated, wild and commercial Gentiana lutea L.

    Science.gov (United States)

    Mustafa, Ahmed M; Caprioli, Giovanni; Ricciutelli, Massimo; Maggi, Filippo; Marín, Rosa; Vittori, Sauro; Sagratini, Gianni

    2015-05-01

    The root of Gentiana lutea L., famous for its bitter properties, is often used in alcoholic bitter beverages, food products and traditional medicine to stimulate the appetite and improve digestion. This study presents a new, fast, and accurate HPLC method using HPLC/ESI-MS and HPLC/DAD for simultaneous analysis of iridoids (loganic acid), secoiridoids (gentiopicroside, sweroside, swertiamarin, amarogentin) and xanthones (isogentisin) in different populations of G.lutea L., cultivated in the Monti Sibillini National Park, obtained wild there, or purchased commercially. Comparison of HPLC/ESI-MS and HPLC/DAD indicated that HPLC/ESI-MS is more sensitive, reliable and selective. Analysis of twenty samples showed that gentiopicroside is the most dominant compound (1.85-3.97%), followed by loganic acid (0.11-1.30%), isogentisin (0.03-0.48%), sweroside (0.05-0.35%), swertiamarin (0.08-0.30%), and amarogentin (0.01-0.07%). The results confirmed the high quality of the G.lutea cultivated in the Monti Sibillini National Park. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Rapid Screening for α-Glucosidase Inhibitors from Gymnema sylvestre by Affinity Ultrafiltration–HPLC-MS

    Directory of Open Access Journals (Sweden)

    Mingquan Guo

    2017-04-01

    Full Text Available Gymnema sylvestre R. Br. (Asclepiadaceae has been known to posses potential anti-diabetic activity, and the gymnemic acids were reported as the main bioactive components in this plant species. However, the specific components responsible for the hypoglycemic effect still remain unknown. In the present study, the in vitro study revealed that the extract of G. sylvestre exhibited significant inhibitory activity against α-glucosidase with IC50 at 68.70 ± 1.22 μg/mL compared to acarbose (positive control at 59.03 ± 2.30 μg/mL, which further indicated the potential anti-diabetic activity. To this end, a method based on affinity ultrafiltration coupled with liquid chromatography mass spectrometry (UF-HPLC-MS was established to rapidly screen and identify the α-glucosidase inhibitors from G. sylvestre. In this way, 9 compounds with higher enrichment factors (EFs were identified according to their MS/MS spectra. Finally, the structure-activity relationships revealed that glycosylation could decrease the potential antisweet activity of sapogenins, and other components except gymnemic acids in G. sylvestre could also be good α-glucosidase inhibitors due to their synergistic effects. Taken together, the proposed method combing α-glucosidase and UF-HPLC-MS presents high efficiency for rapidly screening and identifying potential inhibitors of α-glucosidase from complex natural products, and could be further explored as a valuable high-throughput screening (HTS platform in the early anti-diabetic drug discovery stage.

  4. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    International Nuclear Information System (INIS)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho

    2016-01-01

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic

  5. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho [Dept. of Chemistry and Chemistry Institute for Functional Materials, Pusan National University, Busan (Korea, Republic of)

    2016-12-15

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic.

  6. HPLC-ICP-MS speciation analysis of arsenic in urine of Japanese subjects without occupational exposure.

    Science.gov (United States)

    Hata, Akihisa; Endo, Yoko; Nakajima, Yoshiaki; Ikebe, Maiko; Ogawa, Masanori; Fujitani, Noboru; Endo, Ginji

    2007-05-01

    The toxicity and carcinogenicity of arsenic depend on its species. Individuals living in Japan consume much seafood that contains high levels of organoarsenics. Speciation analysis of urinary arsenic is required to clarify the health risks of arsenic intake. There has been no report of urinary arsenic analysis in Japan using high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). We performed speciation analysis of urinary arsenic for 210 Japanese male subjects without occupational exposure using HPLC-ICP-MS. The median values of urinary arsenics were as follows: sodium arsenite (AsIII), 3.5; sodium arsenate (AsV), 0.1; monomethylarsonic acid (MMA), 3.1; dimethylarsinic acid (DMA), 42.6; arsenobetaine (AsBe), 61.3; arsenocholine, trimethylarsine oxide, and unidentified arsenics (others), 5.2; and total arsenic (total As), 141.3 microgAs/l. The median creatinine-adjusted values were as follows: AsIII, 3.0; AsV, 0.1; MMA, 2.6; DMA, 35.9; AsBe, 52.1; others 3.5; and total As, 114.9 microgAs/g creatinine. Our findings indicate that DMA and AsBe levels in Japan are much higher than those found in Italian and American studies. It appears that the high levels of DMA and AsBe observed in Japan may be due in part to seafood intake. ACGIH and DFG set the BEI and BAT values for occupational arsenic exposure as 35 microgAs/l and 50 microgAs/l, respectively, using the sum of inorganic arsenic (iAs), MMA, and DMA. In the general Japanese population, the sums of these were above 50 microgAs/l in 115 (55%) samples. We therefore recommend excluding DMA concentration in monitoring of iAs exposure.

  7. Determination of 5-fluorouracil in plasma with HPLC-tandem mass spectrometry

    NARCIS (Netherlands)

    van Kuilenburg, A. B. P.; van Lenthe, H.; Maring, J. G.; van Gennip, A. H.

    2006-01-01

    In this article, we describe a fast and specific method to measure 5FU with HPLC tandem-mass spectrometry. Reversed-phase HPLC was combined with electrospray ionization tandem mass spectrometry and detection was performed by multiple-reaction monitoring. Stable-isotope-labeled 5FU (1,3-15N2-5FU) was

  8. Theoretische en practische aspecten van het gebruik van micro-HPLC

    NARCIS (Netherlands)

    de Fluiter P; Jansen EHJM

    1992-01-01

    A practical and theoretical approach for the implementation of micro high performance liquid chromatography (HPLC) is described. A new simple and rapid test procedure was developed in wich a HPLC system can be validated for its suitability for micro-bore columns. It appeared that the detector

  9. Size exclusion HPLC of proteins for evaluation of durum wheat quality

    Science.gov (United States)

    The present research aimed to assess size exclusion HPLC (SE-HPLC) in protein molecular weight distribution determination for quality evaluation of durum semolina. Semolina samples were milled from 13 durum genotypes grown at 7 locations in 2009 and 2010 in ND. Sodium dodecyl sulfate (SDS) buffer ...

  10. Chromatic regulation in cyanobacterium as studies by HPLC quantitation of photosynthetic pigments. Kogosei shikiso no HPLC teiryo ni motozuku ranso no hikari tekio process tsuiseki

    Energy Technology Data Exchange (ETDEWEB)

    Maeda, H.; Watanabe, T. (The Univ. Tokyo, Tokyo (Japan). Inst. of Industrial Science)

    1991-08-01

    Plants higher than Cyanobacterium have two kinds of resction centers(RC) which convert photon energy to a flow of electrons and whose photosensitive spectral regions are slightly deviated from each other. In the photosynthetic process, the ratio of numbers between these two kinds of reaction centers is adaptively varied so as to allow the overall flow of electrons to proceed in a well-balanced manner. It is important to rapidly and exactly determine the ratio of RC numbers between the two photochemical systems in order to investigate such photoadaptive process. The report describes the quantitative determination using high performance liquid chromatography(HPLC) for this purpose. Pigments were extracted from Cyanobacteria which are in different adaptive processes brought by being cultured in the environments differing in the quantity of light or in the environment of varying quantity of light, and subjected to quantitave determination in consideration of the fact that the reaction centers, I and II, have the respective special kinds of chlorophyl derivatives Chl-a, Chl-a{prime}. As the results, it was confirmed that validity can be given to the estimation of the numbers of reaction centers in terms of the quantities of Chl-a and Chl-a prime and the proposed method is drastically faster and simpler than the conventional methods. 14 refs., 5 figs..

  11. [Study on the fingerprint of Morus alba from different habitats by HPLC].

    Science.gov (United States)

    Chen, Cheng; Li, Hong-Bo; Wang, Liu-Ping; Li, Yun-Rong; Xin, Ning

    2012-12-01

    To establish HPLC fingerprint of Morus alba from different habitats by HPLC and provide basis for its quality control. HPLC analysis was performed on an Agilent XDB C18 Column (4.6 mm x 250 mm, 5 microm), gradient eluted composed of acetonitrile and 0.3% phosphate acid. The column temperature was set at 35 degrees C and the flow rate was 0.5 mL/min. The detective wavelength was 290 nm. The HPLC fingerprint for 10 batches of Morus alba was studied on their similarity. There were twelve common peaks in the fingerprint. The similarity of 7 batches was above 0.9 and the other batches had low similarity. The HPLC fingerprint can be used for quality control of Morus alba with high characteristics and specificity.

  12. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Directory of Open Access Journals (Sweden)

    Michel D. Santos

    2008-01-01

    Full Text Available This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules.

  13. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    International Nuclear Information System (INIS)

    Santos, Michel D.; Lopes, Norberto P.; Iamamoto, Yassuko

    2008-01-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  14. HPLC-ESI-MS/MS analysis of oxidized di-caffeoylquinic acids generated by metalloporphyrin-catalyzed reactions

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Michel D.; Lopes, Norberto P. [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Fisica e Quimica]. E-mail: npelopes@fcfrp.usp.br; Iamamoto, Yassuko [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas. Dept. de Quimica

    2008-07-01

    This paper reports an HPLC-ESI-MS/MS investigation on the oxidation of 3,5- and 4,5- dicaffeoylquinic acid using iron(III) tetraphenylporphyrin chloride as catalyst. Two major mono-oxidised products of the quinic acid moiety have been identified for both compounds. However, only the 4,5-derivative afforded two different tri-oxo products. Thus, it seems that the oxidation pattern depends on the number and positions of the caffeic acid moieties present in caffeoylquinic acid molecules. (author)

  15. Stability-Indicating TLC-Densitometric and HPLC Methods for the Simultaneous Determination of Piracetam and Vincamine in the Presence of Their Degradation Products.

    Science.gov (United States)

    Ahmed, Amal B; Abdelrahman, Maha M; Abdelwahab, Nada S; Salama, Fathy M

    2016-11-01

    Newly established TLC-densitometric and RP-HPLC methods were developed and validated for the simultaneous determination of Piracetam (PIR) and Vincamine (VINC) in their pharmaceutical formulation and in the presence of PIR and VINC degradation products, PD and VD, respectively. The proposed TLC-densitometric method is based on the separation and quantitation of the studied components using a developing system that consists of chloroform-methanol-glacial acetic acid-triethylamine (8 + 2 + 0.1 + 0.1, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 230 nm. On the other hand, the developed RP-HPLC method is based on the separation of the studied components using an isocratic elution of 0.05 M KH2PO4 (containing 0.1% triethylamine adjusted to pH 3 with orthophosphoric acid)-methanol (95 + 5, v/v) on a C8 column at a flow rate of 1 mL/min with diode-array detection at 230 nm. The developed methods were validated according to International Conference on Harmonization guidelines and demonstrated good accuracy and precision. Moreover, the developed TLC-densitometric and RP-HPLC methods are suitable as stability-indicating assay methods for the simultaneous determination of PD and VD either in bulk powder or pharmaceutical formulation. The results were statistically compared with those obtained by the reported RP-HPLC method using t- and F-tests.

  16. A simple micro-batch ion-exchange resin extraction method coupled with reverse-phase HPLC (MBRE-HPLC) to quantify lactoferrin in raw and heat-treated bovine milk.

    Science.gov (United States)

    Pochet, Sylvie; Arnould, Céline; Debournoux, Perrine; Flament, Jocelyne; Rolet-Répécaud, Odile; Beuvier, Eric

    2018-09-01

    Lactoferrin is an iron-binding cationic glycoprotein (pI = 8.7) beneficial for mammal health, especially udder and milk preservation. A new simple two-step method of quantification was developed. Lactoferrin in 1 mL of bovine skim milk was first adsorbed onto 100 mg of macroporous sulfonated-resin at pH 6.8 by rotary stirring for 90 min at 20-25 °C. After washing the resin, lactoferrin was desorbed using 1 mL of 2 M NaCl containing phenylalanine as a dilution marker, then fully resolved and quantified by RP-HPLC at 220 nm using a wide-bore C4 silica column. This robust, inexpensive and flexible method improves selectivity (no protein interference) and sensitivity compared to previous HPLC methods. In-laboratory validation demonstrated its linearity (25 to 514 µg Lf mL -1 ), accuracy (110 to 98% recovery), and precision (<4%), which were comparable to immuno-based methods. The results for individual raw cow's milk were strongly correlated with results using an ELISA test. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. Applications of HPLC/MS in the analysis of traditional Chinese medicines

    Science.gov (United States)

    Li, Miao; Hou, Xiao-Fang; Zhang, Jie; Wang, Si-Cen; Fu, Qiang; He, Lang-Chong

    2012-01-01

    In China, traditional Chinese medicines (TCMs) have been used in clinical applications for thousands of years. The successful hyphenation of high-Performance liquid chromatography (HPLC) and mass spectrometry (MS) has been applied widely in TCMs and biological samples analysis. Undoubtedly, HPLC/MS technique has facilitated the understanding of the treatment mechanism of TCMs. We reviewed more than 350 published papers within the last 5 years on HPLC/MS in the analysis of TCMs. The present review focused on the applications of HPLC/MS in the component analysis, metabolites analysis, and pharmacokinetics of TCMs etc. 50% of the literature is related to the component analysis of TCMs, which show that this field is the most populär type of research. In the metabolites analysis, HPLC coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry has been demonstrated to be the powerful tool for the characterization of structural features and fragmentation behavior patterns. This paper presented a brief overview of the applications of HPLC/MS in the analysis of TCMs. HPLC/MS in the fingerprint analysis is reviewed elsewhere. PMID:29403684

  18. HPLC analysis of prostaglandin metabolites plasma from irradiated rats

    International Nuclear Information System (INIS)

    Walden, T.L. Jr.; Catravas, G.N.

    1985-01-01

    The authors used RP-HPLC to quantitatively and qualitatively evaluate the PG metabolites in the plasma of rats during the first 24 hrs following a 10 Gy whole body dose of cobalt 60 gamma rays. The PGs and other arachidonic acid metabolites in plasma were extracted and then covalently attached to a fluroescent dye to enhance detection. A number of PGs and their metabolites were observed in the irradiated sample, including: 13,14 dihydro -15 keto PGE/sub 2/ and 13,14, dihydro -15 keto PGF/sub 2/, and their respective precursors, PGE/sub 2/ and PGF/sub 2/. The two major compounds present in the plasma samples were 13,14 dihydro -15 keto PFG/sub 2/ and another compound which is as yet unidentified. The levels of the individual PGs within a sample varied with time after irradiation, and the time at which a PG reached a peak level in the plasma depended on the particular PG in question. 13,14 dihdyro -15 keto PGD/sub 2/ was observed to reach a peak plasma concentration at 6 hours postirradiation, and at that time was at least 20 times higher than control levels

  19. [HPLC Specific Fingerprint of Alcohol Extract of Andrographis paniculata].

    Science.gov (United States)

    Liu, Fei-fei; Fan, Chun-lin; Huang, Xiao-jun; Wang, Gui-yang; Wang, Ying; Ye, Wen-cai

    2015-07-01

    To establish the specific fingerprint of alcohol extract of Andrographis paniculata by HPLC. The analysis was performed on Cosmosil 5C18 -MS-II (250 mm x 4. 6 mm, 5 µm) column, with gradient phase consisting of acetonitrile and water at the flow rate of 1. 0 mL/min. The UV detection wavelength was set at 225 nm, and column temperature was 30 °C. The specific fingerprint chromatogram was established and seven common peaks were identified by comparison with the reference standards and LC-MS. The relative retention times were 1. 00 (No. 1, andrographolide), 1. 04 (No. 2, deoxyandrographoside), 1. 07 (No. 3, isoandrographolide), 1. 10 (No. 4, 14-deoxy-11, 12-didehydroandrographoside), 1. 50 (No. 5, neoandrographolide), 1. 75 ( No. 6, deoxyandrographolide) and 1. 79 (No. 7, dehydroandrographolide). The method is simple and reproducible with high precision, which can provide the basis for the quality control and evaluation of alcohol extract of Andrographis paniculata and its preparations.

  20. Measurement of purine derivatives and creatinine in urine by HPLC

    International Nuclear Information System (INIS)

    Piani, B.; Fabro, C.; Susmel, P.

    2004-01-01

    Two HPLC methods to measure the purine derivatives (PD, including allantoin, uric acid, hypoxanthine and xanthine) and creatinine content in urine are described. PD separation and quantification were achieved using two Spherisorb ODS 2 reversed phase columns connected in series (4.6 x 250 mm) and a Spherisorb ODS 2 Waters pre-column and a Perkin Elmer pump with an auto sampler. The mobile phase was NH 4 H 2 PO 4 :NH 4 H 2 PO 4 -acetonitrile (80:20), which was used at a flow rate of 0.8 ml/min and the detection wavelength was at 190 nm. The average recoveries of standard compounds added to urine samples were satisfactory (92-106%) and the low detection limits (0.7-3.4 μM) permitted the precise determination of these compounds in urine. Separation and quantification of creatinine was achieved using one Spherisorb ODS 2 reversed phase column (4.6 x 250 mm) and one Spherisorb ODS 2 Waters pre-column and a Perkin Elmer pump with an auto sampler. The mobile phase was NH 4 H 2 PO 4 :NH 4 H 2 PO 4 -acetonitrile (80:20), used at a flow rate of 1.00 ml/min and the detection was at 190 nm. The mean recovery (3 measurements) of standard solution added to urine samples was 101%; detection limit was 7.9 μM. (author)

  1. New validated method for piracetam HPLC determination in human plasma.

    Science.gov (United States)

    Curticapean, Augustin; Imre, Silvia

    2007-01-10

    The new method for HPLC determination of piracetam in human plasma was developed and validated by a new approach. The simple determination by UV detection was performed on supernatant, obtained from plasma, after proteins precipitation with perchloric acid. The chromatographic separation of piracetam under a gradient elution was achieved at room temperature with a RP-18 LiChroSpher 100 column and aqueous mobile phase containing acetonitrile and methanol. The quantitative determination of piracetam was performed at 200 nm with a lower limit of quantification LLQ=2 microg/ml. For this limit, the calculated values of the coefficient of variation and difference between mean and the nominal concentration are CV%=9.7 and bias%=0.9 for the intra-day assay, and CV%=19.1 and bias%=-7.45 for the between-days assay. For precision, the range was CV%=1.8/11.6 in the intra-day and between-days assay, and for accuracy, the range was bias%=2.3/14.9 in the intra-day and between-days assay. In addition, the stability of piracetam in different conditions was verified. Piracetam proved to be stable in plasma during 4 weeks at -20 degrees C and for 36 h at 20 degrees C in the supernatant after protein precipitation. The new proposed method was used for a bioequivalence study of two medicines containing 800 mg piracetam.

  2. Identification of Sulfanilamide, Phenazone, and Lidocaine hydrochloride by HPLC Technique

    International Nuclear Information System (INIS)

    Noaba, R.

    2009-01-01

    A sensitive and accurate method was developed for the analysis of sulfanilamide, phenazone, and lidocaine hydrochloride content in pure form and pharmaceutical preparations using HPLC technique. Analysis was performed on column had the following specifications: SHIM-PACK CLC(M) C18(100A 0 , 5μm, 4.6 x 250 mm). And mobile phase consisting of tow phases: the first was methanol, the second consisting of pure form of [water, icy acetic acid, triethylamine in rate (240: 7: 3 v/v/v) respectively], and the two phases were mixed in rate (20:80) respectively, flow rate was 1.5 ml/min, at temperature 300 C, and detector in the ultraviolet range at wavelength 254 nm, consequently. We could separate and determinate the studied compounds in its mixtures, and reached to excellent linearity for each one with correlation coefficients equivalent to (0.9999). This supposed method was applied on prepared samples and pharmaceutical preparation contains of the three studied compounds. The relative standard deviations RSD (n=5) was smaller than (1.99%) for prepared samples and (2.11%) for the pharmaceutical preparation. So this method proved to be sensitive, accurate, is useful for quantitative control of pharmaceutical products. (author)

  3. HPLC retention thermodynamics of grape and wine tannins.

    Science.gov (United States)

    Barak, Jennifer A; Kennedy, James A

    2013-05-08

    The effect of grape and wine tannin structure on retention thermodynamics under reversed-phase high-performance liquid chromatography conditions on a polystyrene divinylbenzene column was investigated. On the basis of retention response to temperature, an alternative retention factor was developed to approximate the combined temperature response of the complex, unresolvable tannin mixture. This alternative retention factor was based upon relative tannin peak areas separated by an abrupt change in solvent gradient. Using this alternative retention factor, retention thermodynamics were calculated. Van't Hoff relationships of the natural log of the alternative retention factor against temperature followed Kirchoff's relationship. An inverse quadratic equation was fit to the data, and from this the thermodynamic parameters for tannin retention were calculated. All tannin fractions exhibited exothermic, spontaneous interaction, with enthalpy-entropy compensation observed. Normalizing for tannin size, distinct tannin compositional effects on thermodynamic parameters were observed. The results of this study indicate that HPLC can be valuable for measuring the thermodynamics of tannin interaction with a hydrophobic surface and provides a potentially valuable alternative to calorimetry. Furthermore, the information gathered may provide insight into understanding red wine astringency quality.

  4. Development of a HPLC method for determination of four UV filters in sunscreen and its application to skin penetration studies.

    Science.gov (United States)

    Souza, Carla; Maia Campos, Patrícia M B G

    2017-12-01

    This study describes the development, validation and application of a high-performance liquid chromatography (HPLC) method for the simultaneous determination of the in vitro skin penetration profile of four UV filters on porcine skin. Experiments were carried out on a gel-cream formulation containing the following UV filters: diethylamino hydroxybenzoyl hexyl benzoate (DHHB), bis-ethylhexyloxyphenol methoxyphenyl triazine (BEMT), methylene bis-benzotriazolyl tetramethylbutylphenol (MBBT) and ethylhexyl triazone (EHT). The HPLC method demonstrated suitable selectivity, linearity (10.0-50.0 μg/mL), precision, accuracy and recovery from porcine skin and sunscreen formulation. The in vitro skin penetration profile was evaluated using Franz vertical diffusion cells for 24 h after application on porcine ear skin. None of the UV filters penetrated the porcine skin. Most of them stayed on the skin surface (>90%) and only BEMT, EHT and DHHB reached the dermis plus epidermis layer. These results are in agreement with previous results in the literature. Therefore, the analytical method was useful to evaluate the in vitro skin penetration of the UV filters and may help the development of safer and effective sunscreen products. Copyright © 2017 John Wiley & Sons, Ltd.

  5. Biological variability dominates and influences analytical variance in HPLC-ECD studies of the human plasma metabolome

    Directory of Open Access Journals (Sweden)

    Willett Walter C

    2007-11-01

    Full Text Available Abstract Background Biomarker-based assessments of biological samples are widespread in clinical, pre-clinical, and epidemiological investigations. We previously developed serum metabolomic profiles assessed by HPLC-separations coupled with coulometric array detection that can accurately identify ad libitum fed and caloric-restricted rats. These profiles are being adapted for human epidemiology studies, given the importance of energy balance in human disease. Methods Human plasma samples were biochemically analyzed using HPLC separations coupled with coulometric electrode array detection. Results We identified these markers/metabolites in human plasma, and then used them to determine which human samples represent blinded duplicates with 100% accuracy (N = 30 of 30. At least 47 of 61 metabolites tested were sufficiently stable for use even after 48 hours of exposure to shipping conditions. Stability of some metabolites differed between individuals (N = 10 at 0, 24, and 48 hours, suggesting the influence of some biological factors on parameters normally considered as analytical. Conclusion Overall analytical precision (mean median CV, ~9% and total between-person variation (median CV, ~50–70% appear well suited to enable use of metabolomics markers in human clinical trials and epidemiological studies, including studies of the effect of caloric intake and balance on long-term cancer risk.

  6. HPLC and ELISA analyses of larval bile acids from Pacific and western brook lampreys

    Science.gov (United States)

    Yun, S.-S.; Scott, A.P.; Bayer, J.M.; Seelye, J.G.; Close, D.A.; Li, W.

    2003-01-01

    Comparative studies were performed on two native lamprey species, Pacific lamprey (Lampetra tridentata) and western brook lamprey (Lampetra richardsoni) from the Pacific coast along with sea lamprey (Petromyzon marinus) from the Great Lakes, to investigate their bile acid production and release. HPLC and ELISA analyses of the gall bladders and liver extract revealed that the major bile acid compound from Pacific and western brook larval lampreys was petromyzonol sulfate (PZS), previously identified as a migratory pheromone in larval sea lamprey. An ELISA for PZS has been developed in a working range of 20pg-10ng per well. The tissue concentrations of PZS in gall bladder were 127.40, 145.86, and 276.96??g/g body mass in sea lamprey, Pacific lamprey, and western brook lamprey, respectively. Releasing rates for PZS in the three species were measured using ELISA to find that western brook and sea lamprey released PZS 20 times higher than Pacific lamprey did. Further studies are required to determine whether PZS is a chemical cue in Pacific and western brook lampreys. ?? 2003 Elsevier Inc. All rights reserved.

  7. High-Grade Leiomyosarcoma Arising in a Previously Replanted Limb

    Directory of Open Access Journals (Sweden)

    Tiffany J. Pan

    2015-01-01

    Full Text Available Sarcoma development has been associated with genetics, irradiation, viral infections, and immunodeficiency. Reports of sarcomas arising in the setting of prior trauma, as in burn scars or fracture sites, are rare. We report a case of a leiomyosarcoma arising in an arm that had previously been replanted at the level of the elbow joint following traumatic amputation when the patient was eight years old. He presented twenty-four years later with a 10.8 cm mass in the replanted arm located on the volar forearm. The tumor was completely resected and pathology examination showed a high-grade, subfascial spindle cell sarcoma diagnosed as a grade 3 leiomyosarcoma with stage pT2bNxMx. The patient underwent treatment with brachytherapy, reconstruction with a free flap, and subsequently chemotherapy. To the best of our knowledge, this is the first case report of leiomyosarcoma developing in a replanted extremity. Development of leiomyosarcoma in this case could be related to revascularization, scar formation, or chronic injury after replantation. The patient remains healthy without signs of recurrence at three-year follow-up.

  8. Application of Pattern Recognition Method for Color Assessment of Oriental Tobacco based on HPLC of Polyphenols

    Directory of Open Access Journals (Sweden)

    Dagnon S

    2014-12-01

    Full Text Available The color of Oriental tobaccos was organoleptically assayed, and high performance liquid chromatography (HPLC of polyphenols was performed. The major tobacco polyphenols (chlorogenic acid, its isomers, and rutin, as well as scopoletin and kaempferol-3-rutinoside were quantified. HPLC polyphenol profiles were processed by pattern recognition method (PRM, and the values of indexes of similarity (Is,% between the cultivars studied were determined. It was shown that data from organoleptic color assessment and from PRM based on HPLC profiles of polyphenols of the cultivars studied are largely compatible. Hence, PRM can be suggested as an additional tool for objective color evaluation and classification of Oriental tobacco.

  9. Electrochemically Pretreated Carbon Microfiber Electrodes as Sensitive HPLC-EC Detectors

    Directory of Open Access Journals (Sweden)

    Zdenka Bartosova

    2012-01-01

    Full Text Available The paper focuses on the analysis and detection of electroactive compounds using high-performance liquid chromatography (HPLC combined with electrochemical detection (EC. The fabrication and utilization of electrochemically treated carbon fiber microelectrodes (CFMs as highly sensitive amperometric detectors in HPLC are described. The applied pretreatment procedure is beneficial for analytical characteristics of the sensor as demonstrated by analysis of the model set of phenolic acids. The combination of CFM with separation power of HPLC technique allows for improved detection limits due to unique electrochemical properties of carbon fibers. The CFM proved to be a promising tool for amperometric detection in liquid chromatography.

  10. Determination of sulfonamides and trimethoprim using high temperature HPLC with simultaneous temperature and solvent gradient.

    Science.gov (United States)

    Giegold, Sascha; Teutenberg, Thorsten; Tuerk, Jochen; Kiffmeyer, Thekla; Wenclawiak, Bernd

    2008-10-01

    A fast HPLC method for the analysis of eight selected sulfonamides (SA) and trimethoprim has been developed with the use of high temperature HPLC. The separation could be achieved in less than 1.5 min on a 50 mm sub 2 microm column with simultaneous solvent and temperature gradient programming. Due to the lower viscosity of the mobile phase and the increased mass transfer at higher temperatures, the separation could be performed on a conventional HPLC system obtaining peak widths at half height between 0.6 and 1.3 s.

  11. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  12. HPLC-RID-DAD-MS analysis of 18F-Fluorodeoxyglucose

    International Nuclear Information System (INIS)

    Macasek, F.; Buriova, E.; Bruder, P.

    2001-01-01

    Objective of new method of FDG analysis development is to replace existing tests by more complex assay. In this work, a liquid chromatography/refractive index detector/diode array detector/mass spectrometric detector combination (HPLC/RID/DAD/MSD) was used for development of a complex routine technique. Optimization of the HPLC/MS analysis was performed investigating MSD analytical signal as a function of various eluent composition. HPLC-RID-DAD-MSD analysis has potentiality of a complex quality control of radiopharmaceuticals, FDG in particular, providing information about: isotope composition; chemical composition; biochemical composition; radiation stability; pharmacodynamics. (author)

  13. Quantification of Catechin in Leaves and Stems of Malaysian Uncaria Gambir (Hunter) ROXB. by HPLC-DAD

    International Nuclear Information System (INIS)

    Nurliayana Ibrahim; Nurul Zulaikha Mohd Yusoff; Rohaya Ahmad; Rohaya Ahmad

    2016-01-01

    Recently, we reported the isolation of a novel flavonoid named uncariechin along with epicatechin and epiafzelechin from the leaf extract of Uncaria longiflora variety pteropoda (Miq.) Ridsd. of the family Rubiaceae. Continuing our investigation on the Uncaria genus, the identification and quantification of its phytoconstituents was carried out. The species of particular interest is the Malaysian Uncaria gambir. This species is distributed mainly in Malaysia and Indonesia and has been cultivated for the flavonoid catechin in Indonesia. Hence, the objective of this study is to determine the quantity of catechin in hexane (Hx), dichloromethane (DCM) and methanol (MeOH) extracts in both stem and leaf parts of the plant via HPLC-DAD. Our findings indicate that catechin is present in higher amounts in the MeOH extract [8.64 % (leaves); 5.12 % (stems)] compared to the DCM extract [0.77 % (leaves); 0.92 % (stems)] with no catechin found in the hexane extract. This is the first report of the quantification of catechin from Malaysian U. gambir using HPLC-DAD. The method can be used for the quantification of flavonoids from other Uncaria and related genus and is useful for targeted isolation of interest flavonoids. (author)

  14. Pregnancy and variations of carbohydrate-deficient transferrin levels measured by the candidate reference HPLC method.

    Science.gov (United States)

    Bianchi, Vincenza; Ivaldi, Alessandra; Raspagni, Alessia; Arfini, Carlo; Vidali, Matteo

    2011-01-01

    Contrasting data are available on the diagnostic accuracy of carbohydrate-deficient transferrin (CDT) during pregnancy. These differences may depend in part on how CDT was evaluated and expressed. Here, we report on variations of CDT levels in pregnant women using the high performance liquid chromatography (HPLC) candidate reference method. Alanine aminotransferase, aspartate aminotransferase, gamma-glutamyltransferase, mean corpuscular volume, serum transferrin, urine and serum ethyl glucuronide and CDT were measured in 64 women, self-reporting as non-alcohol abusers (age: median 34, IQR: 28-38), at different stages of normal pregnancy (gestational weeks: median 28, IQR: 8-33). CDT was expressed as percentage of disialotransferrin to total transferrin (%CDT). Transferrin was associated with both %CDT (r = 0.66; P pregnancy trimester (first trimester: mean 1.01% (SD 0.19); second trimester: 1.30% (SD 0.14); third trimester: 1.53% (SD 0.22); ANOVA P pregnancy trimesters (P pregnancy and CDT could be more complex. The diagnostic accuracy of CDT for detecting alcohol abuse in a legal context may be limited in pregnant women and the effect of gestational age should be considered.

  15. 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.; Oliveira, Tiago F.; 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...

  16. Determining the degradation efficiency and mechanisms of ethyl violet using HPLC-PDA-ESI-MS and GC-MS

    Directory of Open Access Journals (Sweden)

    Chung Wen-Hsin

    2012-06-01

    Full Text Available Abstract Background The discharge of wastewater that contains high concentrations of reactive dyes is a well-known problem associated with dyestuff activities. In recent years, semiconductor photocatalysis has become more and more attractive and important since it has a great potential to contribute to such environmental problems. One of the most important aspects of environmental photocatalysis is in the selection of semiconductor materials like ZnO and TiO2, which are close to being two of the ideal photocatalysts in several respects. For example, they are relatively inexpensive, and they provide photo-generated holes with high oxidizing power due to their wide band gap energy. In this work, nanostructural ZnO film on the Zn foil of the Alkaline-Manganese Dioxide-Zinc Cell was fabricated to degrade EV dye. The major innovation of this paper is to obtain the degradation mechanism of ethyl violet dyes resulting from the HPLC-PDA-ESI-MS analyses. Results The fabrication of ZnO nanostructures on zinc foils with a simple solution-based corrosion strategy and the synthesis, characterization, application, and implication of Zn would be reported in this study. Other objectives of this research are to identify the reaction intermediates and to understand the detailed degradation mechanism of EV dye, as model compound of triphenylmethane dye, with active Zn metal, by HPLC-ESI-MS and GC-MS. Conclusions ZnO nanostructure/Zn-foils had an excellent potential for future applications on the photocatalytic degradation of the organic dye in the environmental remediation. The intermediates of the degradation process were separated and characterized by the HPLC-PDA-ESI-MS and GC-MS, and twenty-six intermediates were characterized in this study. Based on the variation of the amount of intermediates, possible degradation pathways for the decolorization of dyes are also proposed and discussed.

  17. Comparative study of the hypocholesterolemic, antidiabetic effects of four agro-waste Citrus peels cultivars and their HPLC standardization

    Directory of Open Access Journals (Sweden)

    Nesrin M. Fayek

    Full Text Available ABSTRACT Citrus is an economically important fruit for Egypt, but its peel also is one of the major sources of agricultural waste. Due to its fermentation, this waste causes many economic and environmental problems. Therefore it is worthwhile to investigate ways to make use of this citrus waste generated by the juice industry. This study was aimed to explore the hypocholesterolemic, antidiabetic activities of four varieties of citrus peels agrowastes, to isolate the main flavonoids in the active fractions and to quantify them by HPLC method for nutraceutical purposes. All the tested samples of the agro-waste Citrus fruits peels showed significant decrease in cholesterol, triacylglyceride and glucose. The most decrease in cholesterol level was observed by mandarin peels aqueous homogenate and its hexane fraction (59.3% and 56.8%, respectively reaching the same effect as the reference drug used (54.7%. Mostly, all samples decrease triacylglyceride (by 36%–80.6% better than the reference drug used (by 35%, while, glucose was decreased (by 71.1%–82.8 and 68.6%–79.6%, respectively mostly by the aqueous homogenates (except lime and alcoholic extracts (except mandarin of Citrus fruits peels better than the reference drug used (by 68.3%. All the isolated pectin, from the four cultivars, has significant effect on the three parameters. The comparative HPLC rapid quantification of nobiletin in the different by-product citrus varieties hexane fractions revealed that nobiletin is present in higher concentration in mandarin (10.14% than the other species. Nobiletin and 4′,5,7,8-tetramethoxy flavone were isolated from mandarin peels hexane fraction by chromatographic fractionation. This is the first report of the comparative HPLC quantification of nobiletin and biological studies of different citrus peels species as agro-waste products. Based on these results, we suggest the possibility that Citrus fruits peels may be considered as an antidiabetic and

  18. Simultaneous qualification and quantification of baccharane glycosides in Impatientis Semen by HPLC-ESI-MSD and HPLC-ELSD.

    Science.gov (United States)

    Li, Hui-Jun; Yu, Jun-Jie; Li, Ping

    2011-03-25

    This study presents a high performance liquid chromatography (HPLC) with electrospray ionization mass spectrometric detection (ESI-MSD) and evaporative light scattering detection (ELSD) method for the simultaneous qualification and quantification of eight major baccharane glycosides, namely hosenlosides A, B, C, F, G, K, L, and M in Impatientis Semen, a Chinese herbal medicine derived from the seeds of Impatiens balsamina L. In order to achieve optimum performance, several extraction parameters (including extraction solvent, extraction mode, extraction time) were optimized. The baccharane glycosides were separated on a Shim-pack CLC-ODS column with gradient elution of water and methanol. Temperature for the ELSD drift tube was set at 98°C and the nitrogen flow rate was 2.7l/min. The unambiguous identities of the analytes were realized by comparing retention times and mass data with those of reference compounds. The developed method was fully validated in terms of linearity, sensitivity, precision, repeatability, recovery as well as robustness, and subsequently applied to evaluate the quality of 14 batches of Impatientis Semen commercial samples from different collections. Copyright © 2010 Elsevier B.V. All rights reserved.

  19. HPLC determination of betamethasone and prednisolone in urine samples using monolithic column

    International Nuclear Information System (INIS)

    Abro, K.; Memon, N.; Bhanger, M.I.

    2011-01-01

    A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification of prednisolone and betamethasone in urine samples. A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification

  20. Online identification of chlorogenic acids, sesquiterpene lactones, and flavonoids in the Brazilian arnica Lychnophora ericoides Mart. (Asteraceae) leaves by HPLC-DAD-MS and HPLC-DAD-MS/MS and a validated HPLC-DAD method for their simultaneous analysis.

    Science.gov (United States)

    Gobbo-Neto, Leonardo; Lopes, Norberto P

    2008-02-27

    Lychnophora ericoides Mart. (Asteraceae, Vernonieae) is a plant, endemic to Brazil, with occurrence restricted to the "cerrado" biome. Traditional medicine employs alcoholic and aqueous-alcoholic preparations of leaves from this species for the treatment of wounds, inflammation, and pain. Furthermore, leaves of L. ericoides are also widely used as flavorings for the Brazilian traditional spirit "cachaça". A method has been developed for the extraction and HPLC-DAD analysis of the secondary metabolites of L. ericoides leaves. This analytical method was validated with 11 secondary metabolites chosen to represent the different classes and polarities of secondary metabolites occurring in L. ericoides leaves, and good responses were obtained for each validation parameter analyzed. The same HPLC analytical method was also employed for online secondary metabolite identification by HPLC-DAD-MS and HPLC-DAD-MS/MS, leading to the identification of di- C-glucosylflavones, coumaroylglucosylflavonols, flavone, flavanones, flavonols, chalcones, goyazensolide, and eremantholide-type sesquiterpene lactones and positional isomeric series of chlorogenic acids possessing caffeic and/or ferulic moieties. Among the 52 chromatographic peaks observed, 36 were fully identified and 8 were attributed to compounds belonging to series of caffeoylferuloylquinic and diferuloylquinic acids that could not be individualized from each other.

  1. Analysis of sesquiterpene lactones, lignans, and flavonoids in wormwood (Artemisia absinthium L.) using high-performance liquid chromatography (HPLC)-mass spectrometry, reversed phase HPLC, and HPLC-solid phase extraction-nuclear magnetic resonance.

    Science.gov (United States)

    Aberham, Anita; Cicek, Serhat Sezai; Schneider, Peter; Stuppner, Hermann

    2010-10-27

    Today, the medicinal use of wormwood (Artemisia absinthium) is enjoying a resurgence of popularity. This study presents a specific and validated high-performance liquid chromatography (HPLC)-diode array detection method for the simultaneous determination and quantification of bioactive compounds in wormwood and commercial preparations thereof. Five sesquiterpene lactones, two lignans, and a polymethoxylated flavonoid were baseline separated on RP-18 material, using a solvent gradient consisting of 0.085% (v/v) o-phosphoric acid and acetonitrile. The flow rate was 1.0 mL/min, and chromatograms were recorded at 205 nm. The stability of absinthin was tested exposing samples to light, moisture, and different temperatures. Methanolic and aqueous solutions of absinthin were found to be stable for up to 6 months. This was also the case when the solid compound was kept in the refrigerator at -35 °C. In contrast, the colorless needles, when stored at room temperature, turned yellow. Three degradation compounds (anabsin, anabsinthin, and the new dimer 3'-hydroxyanabsinthin) were identified by HPLC-mass spectrometry and HPLC-solid-phase extraction-nuclear magnetic resonance and quantified by the established HPLC method.

  2. [Comparative data regarding two HPLC methods for determination of isoniazid].

    Science.gov (United States)

    Gârbuleţ, Daniela; Spac, A F; Dorneanu, V

    2009-01-01

    For the determination of isoniazide (isonicotinic acid hydrazide - HIN) two different HPLC methods were developed and validated. Both experiments were performed using a Waters 2695 liquid chromatograph and a UV - Waters 2489 detector. The first method (I) used a Nucleosil 100-10 C18 column (250 x 4.6 mm), a mobile phase formed by a mixture of acetonitrile/10(-2) M oxalic acid (80/20) and a flow of 1.5 mL/ min; detection was done at 230 nm. The second method (II) used a Luna 100-5 C18 column (250 x 4.6 mm), a mobile phase formed by a mixture of methanol/acetate buffer, pH = 5.0 (20/ 80), a flow of 1 mL/min; detection was done at 270 nm. Both methods were validated, the correlation coefficients were 0.9998 (I) and 0.9999 (II), the detection limits were 0.6 microg/mL (I) and 0.055 microg/mL (II), the quantitation limits were 1.9 microg/mL (I) and 0.2 microg/ mL (II). There were also studied: the system precision (RSD = 0.1692% (I) and 0.2000% (II)), the method precision (RSD = 1.1844% (I) and 0.6170% (II)) and the intermediate precision (RSD = 1.8058% (I) and 0.5970% (II)). The accuracy was good, the calculated recoveries were 102.66% (I) and 101.36 (II). Both validated methods were applied for HIN determination from tablets with good and comparable results.

  3. Analysis of cesium extracting solvent using GCMS and HPLC

    International Nuclear Information System (INIS)

    White, T.L.; Herman, C.C.; Crump, S.L.; Marinik, A.R.; Lambert, D.P.; Eibling, R.E.

    2007-01-01

    A high-level waste (HLW) remediation process scheduled to begin in 2007 at the Savannah River Site is the Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU). The MCU will use a hydrocarbon solvent (diluent) containing a cesium extractant, a calix[4]arene compound, to extract radioactive cesium from caustic HLW. The resulting decontaminated HLW waste or raffinate will be processed into grout at the Saltstone Production Facility (SPF). The cesium containing CSSX stream will undergo washing with dilute nitric acid followed by stripping of the cesium nitrate into a very dilute nitric acid or the strip effluent stream and the CSSX solvent will be recycled. The Defense Waste Processing Facility (DWPF) will receive the strip effluent stream and immobilize the cesium into borosilicate glass. Excess CSSX solvent carryover from the MCU creates a potential flammability problem during DWPF processing. Bench-scale DWPF process testing was performed with simulated waste to determine the fate of the CSSX solvent components. A simple high performance liquid chromatography (HPLC) method was developed to identify the modifier (which is used to increase Cs extraction and extractant solubility) and extractant within the DWPF process. The diluent and trioctylamine (which is used to suppress impurity effect and ion-pair disassociation) were determined using gas chromatography mass spectroscopy (GCMS). To close the organic balance, two types of sample preparation methods were needed. One involved extracting aqueous samples with methylene chloride or hexane, and the second was capturing the off gas of the DWPF process using carbon tubes and rinsing the tubes with carbon disulfide for analysis. This paper addresses the development of the analytical methods and the bench-scale simulated waste study results. (author)

  4. Which method for quantifying urinary albumin excretion gives what outcome? A comparison of immunonephelometry with HPLC

    NARCIS (Netherlands)

    Brinkman, JW; Bakker, SJL; Gansevoort, RT; Hillege, HL; Kema, IP; Gans, ROB; De Jong, PE; De Zeeuw, D

    2004-01-01

    Background. Microalbuminuria has recently been identified as an independent risk factor for cardiovascular disease in the general population. Immunochemical urinary albumin assays only detect immunoreactive intact albumin. High performance liquid chromatography (HPLC) is able to detect both

  5. HPLC for simultaneous quantification of total ceramide, glucosylceramide, and ceramide trihexoside concentrations in plasma

    NARCIS (Netherlands)

    Groener, Johanna E. M.; Poorthuis, Ben J. H. M.; Kuiper, Sijmen; Helmond, Mariette T. J.; Hollak, Carla E. M.; Aerts, Johannes M. F. G.

    2007-01-01

    BACKGROUND: Simple, reproducible assays are needed for the quantification of sphingolipids, ceramide (Cer), and sphingoid bases. We developed an HPLC method for simultaneous quantification of total plasma concentrations of Cer, glucosylceramide (GlcCer), and ceramide trihexoside (CTH). METHODS:

  6. Automated precolumn derivatization procedures in HPLC for biomedical and clinical applications

    NARCIS (Netherlands)

    Wolf, Johannes Hendrik

    1992-01-01

    This thesis describes three automated precolumn derivatization procedures for the analysis of carboxylic group-containing compounds. After derivatization with a suitable label, the derivatives are separated on reversed-phashed HPLC and detected by fluorescence. ... Zie: Summary

  7. [HPLC fingerprint analysis of flavonoids of phyllanthi fructus from different habitats].

    Science.gov (United States)

    Wang, Fei; Wang, Shuai; Meng, Xian-sheng; Bao, Yong-rui; Zhu, Ying-huan

    2014-11-01

    To establish the HPLC fingerprint of flavonoids of Phyllanthi Fructus from different habitats. HPLC method was adopted. The flavonoids composition of Phyllanthi Fructus from 10 different habitats was determined on an Agilent C, chromatographic column with 0. 5% formic acid water (A)-acetonitrile (B) as the mobile phase in gradient elution under the wavelength of 254 nm. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus were established to evaluate the qualitiy of them. The HPLC fingerprints of flavonoids composition of Phyllanthi Fructus from 10 different habitats were established. 18 common peaks were found and the similarities of them were more than 0. 90 except the ones from Guangxi and Guangdong. The method is simple, accurate and repeatable. It can be used for research and quality control of the effective components in Phyllanthi Fructus.

  8. Development and Validation of a RP-HPLC Method for the ...

    African Journals Online (AJOL)

    Development and Validation of a RP-HPLC Method for the Simultaneous Determination of Rifampicin and a Flavonoid Glycoside - A Novel ... range, accuracy, precision, limit of detection, limit of quantification, robustness and specificity.

  9. Antioxidant, antiinflammatory activities and HPLC analysis of South African Salvia species

    CSIR Research Space (South Africa)

    Kamatou, GGP

    2010-03-01

    Full Text Available -performance liquid chromatography (HPLC) was used to identify various compounds in the extracts. Betulafolientriol oxide and rosmarinic acid were detected in all the species investigated, and rosmarinic acid, carnosic acid, carnosol and oleanolic acid/ursolic acid...

  10. Development and Validation of a Stability-Indicating RP-HPLC ...

    African Journals Online (AJOL)

    Development and Validation of a Stability-Indicating RP-HPLC Method for ... of Paracetamol, Tramadol HCl and Domperidone in a Combined Dosage Form. ... testing, as well as for quality control of the combined drugs in pharmaceutical ...

  11. Cerebral Metastasis from a Previously Undiagnosed Appendiceal Adenocarcinoma

    Directory of Open Access Journals (Sweden)

    Antonio Biroli

    2012-01-01

    Full Text Available Brain metastases arise in 10%–40% of all cancer patients. Up to one third of the patients do not have previous cancer history. We report a case of a 67-years-old male patient who presented with confusion, tremor, and apraxia. A brain MRI revealed an isolated right temporal lobe lesion. A thorax-abdomen-pelvis CT scan showed no primary lesion. The patient underwent a craniotomy with gross-total resection. Histopathology revealed an intestinal-type adenocarcinoma. A colonoscopy found no primary lesion, but a PET-CT scan showed elevated FDG uptake in the appendiceal nodule. A right hemicolectomy was performed, and the specimen showed a moderately differentiated mucinous appendiceal adenocarcinoma. Whole brain radiotherapy was administrated. A subsequent thorax-abdomen CT scan revealed multiple lung and hepatic metastasis. Seven months later, the patient died of disease progression. In cases of undiagnosed primary lesions, patients present in better general condition, but overall survival does not change. Eventual identification of the primary tumor does not affect survival. PET/CT might be a helpful tool in detecting lesions of the appendiceal region. To the best of our knowledge, such a case was never reported in the literature, and an appendiceal malignancy should be suspected in patients with brain metastasis from an undiagnosed primary tumor.

  12. Gastrointestinal tolerability with ibandronate after previous weekly bisphosphonate treatment.

    Science.gov (United States)

    Derman, Richard; Kohles, Joseph D; Babbitt, Ann

    2009-01-01

    Data from two open-label trials (PRIOR and CURRENT) of women with postmenopausal osteoporosis or osteopenia were evaluated to assess whether monthly oral and quarterly intravenous (IV) ibandronate dosing improved self-reported gastrointestinal (GI) tolerability for patients who had previously experienced GI irritation with bisphosphonate (BP) use. In PRIOR, women who had discontinued daily or weekly BP treatment due to GI intolerance received monthly oral or quarterly IV ibandronate for 12 months. The CURRENT subanalysis included women receiving weekly BP treatment who switched to monthly oral ibandronate for six months. GI symptom severity and frequency were assessed using the Osteoporosis Patient Satisfaction Questionnaire. In PRIOR, mean GI tolerability scores increased significantly at month 1 from screening for both treatment groups (oral: 79.3 versus 54.1; IV: 84.4 versus 51.0; p 90% at Month 10). In the CURRENT subanalysis >60% of patients reported improvements in heartburn or acid reflux and >70% indicated improvement in other stomach upset at month 6. Postmenopausal women with GI irritability with daily or weekly BPs experienced improvement in symptoms with extended dosing monthly or quarterly ibandronate compared with baseline.

  13. HPLC Analysis of nine corticosteroids in “natural creams” for atopic eczema

    OpenAIRE

    Ameti, Agim; Poposka, Zaklina; Memeti, Shaban; Shishovska, Maja; Mustafa, Zana; Starkoska, Katerina; Arsova-Sarafinovska, Zorica

    2013-01-01

    Purpose: The aim of the study was to determine whether “natural creams” sold for treatment of childhood atopic eczema illegally contain corticosteroids with a newly developed rapid and simple HPLC analysis with UV detection. Material and Methods: HPLC analysis was performed using a Schimadzu LC-2010 chromatographic system (Schimadzu, Kyoto, Japan) consisting of a LC-20AT Prominence liquid chromatography pump with DGU-20A5 Prominence degasser, a SPD-M20A Prominence Diode Array Detector, and...

  14. Expermental Studies of quantitative evaluation using HPLC and safety of Sweet Bee Venom

    OpenAIRE

    Ki Rok Kwon; Ching Seng Chu; Hee Soo Park; Min Ki Kim; Bae Chun Cha; Eun Lee

    2007-01-01

    Objectives : This study was conducted to carry out quantitative evaluation and safety of Sweet Bee Venom. Methods : Content analysis was done using HPLC, measurement of LD50 was conducted intravenous, subcutaneous, and intra-muscular injection to the ICR mice. Results : 1. According to HPLC analysis, removal of the enzymes containing phospholipase A2 was successfully rendered on Sweet Bee Venom. And analyzing melittin content, Sweet Bee Venom contained 12% more melittin than Bee Venom. ...

  15. Development of HPLC Protocol and Simultaneous Quantification of Four Free Flavonoids from Dracocephalum heterophyllum Benth.

    OpenAIRE

    Numonov, Sodik Rakhmonovich; Qureshi, Muhammad Nasimullah; Aisa, Haji Akber

    2015-01-01

    Quantification of the four flavonoids, namely, luteolin, kaempferol, diosmetin, and chrysosplenetin, has been performed for the first time in 80% ethanolic extract of Dracocephalum heterophyllum B. through HPLC coupled to UV detector after optimization of extracting solvent and chromatographic conditions. Total flavonoids quantified were 0.324 mg/mL of the extract. HPLC analysis delivered contents of the luteolin, kaempferol, diosmetin, and chrysosplenetin as 0.08%, 0.14%, 0.28%, and 0.79% of...

  16. Extraction and Quantitative HPLC Analysis of Coumarin in Hydroalcoholic Extracts of Mikania glomerata Spreng: ("guaco" Leaves

    Directory of Open Access Journals (Sweden)

    Celeghini Renata M. S.

    2001-01-01

    Full Text Available Methods for preparation of hydroalcoholic extracts of "guaco" (Mikania glomerata Spreng. leaves were compared: maceration, maceration under sonication, infusion and supercritical fluid extraction. Evaluation of these methods showed that maceration under sonication had the best results, when considering the ratio extraction yield/extraction time. A high performance liquid chromatography (HPLC procedure for the determination of coumarin in these hydroalcoholic extracts of "guaco" leaves is described. The HPLC method is shown to be sensitive and reproducible.

  17. Extensive characterisation of bioactive phenolic constituents from globe artichoke (Cynara scolymus L.) by HPLC-DAD-ESI-QTOF-MS.

    Science.gov (United States)

    Abu-Reidah, Ibrahim M; Arráez-Román, David; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto

    2013-12-01

    The aim of this work was to characterise the phenolic compounds in artichoke (hearts) by using HPLC coupled to DAD-ESI-QTOF-MS, which proved useful in characterising 61 phenolic and other polar compounds. Notably, of the 61 compounds characterised, 34 new phenolic compounds with their isomers have been tentatively characterised in artichoke for the first time, namely: 3 hydroxybenzoic acids, 17 hydroxycinnamic acids, 4 lignans, 7 flavones, 2 flavonols, and 1 phenol derivative. Moreover, a total of 28 isomers of previously described phenolics have also been detected. The data compiled from the qualitative polyphenol characterisation indicate that the artichoke extract analysed (Blanca de Tudela variety) could be regarded as a bioactive functional food and also as a promising source of antioxidant phenolic compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. HPLC/MS identification of the polyphenols present in an extract of Myrtus communis L. obtained by supercritical fluid extraction

    Directory of Open Access Journals (Sweden)

    Paula Pereira

    2017-12-01

    Full Text Available In this work, we studied an extract obtained by supercritical fluid extraction (SFE using a simpler method of cosolvent (ethanol addition. Instead of using a liquid pump, which is the most common process, the ethanol was directly introduced in the extraction cell, immediately after loading the cell with the plant sample. it was our intent to investigate if this change would have any effect in the composition of the extract obtained. The experimental conditions used were: temperature 48° C, pressure 10 MPa, supercritical fluid (SCF flow rate 130.71dm3h-1 (0.238 kgh-1 and an ethanol volume of 104 cm3. The composition of the extract obtained was different from previous tests, and the compounds identified by HPLC-MS were quinic acid, quinic acid 3,5-di-O-gallate, quinic acid 3,4,5-galloyl, myricetin-galactoside gallate, quercetin-galactoside gallate, quercetin, and myricetin-galactosiderhamnoside.

  19. Detection of mono- and di-hexoses as metabolites of 4-bromoaniline using HPLC-TOF-MS/MS.

    Science.gov (United States)

    Major, H; Castro-Perez, J; Nicholson, J K; Wilson, I D

    2003-08-01

    1. The metabolic fate of 4-bromoaniline (4-BrA) was investigated in rat following intraperitoneal administration at 50 mg kg(-1) using HPLC-TOF-MS/MS. 2. The sensitivity provided by the use of TOF-MS/MS, aided by the distinctive isotope pattern resulting from the presence of the bromine substituent in the molecule, enabled the detection of many previously uncharacterized metabolites in the samples. 3. Several groups of minor metabolites were detected in the urine that corresponded to a number of isomeric hexose and di-hexose-containing conjugates (possibly glucosides and diglucosides) of 4-BrA. 4. As well as hexose and di-hexose conjugates of 4-BrA, several further groups of metabolites that also contained either a sulphamate or sulphate group in addition to the sugar moieties were also detected.

  20. Gastrointestinal tolerability with ibandronate after previous weekly bisphosphonate treatment

    Directory of Open Access Journals (Sweden)

    Richard Derman

    2009-09-01

    Full Text Available Richard Derman1, Joseph D Kohles2, Ann Babbitt31Department of Obstetrics and Gynecology, Christiana Hospital, Newark, DE, USA; 2Roche, Nutley, NJ, USA; 3Greater Portland Bone and Joint Specialists, Portland, ME, USAAbstract: Data from two open-label trials (PRIOR and CURRENT of women with postmenopausal osteoporosis or osteopenia were evaluated to assess whether monthly oral and quarterly intravenous (IV ibandronate dosing improved self-reported gastrointestinal (GI tolerability for patients who had previously experienced GI irritation with bisphosphonate (BP use. In PRIOR, women who had discontinued daily or weekly BP treatment due to GI intolerance received monthly oral or quarterly IV ibandronate for 12 months. The CURRENT subanalysis included women receiving weekly BP treatment who switched to monthly oral ibandronate for six months. GI symptom severity and frequency were assessed using the Osteoporosis Patient Satisfaction Questionnaire™. In PRIOR, mean GI tolerability scores increased significantly at month 1 from screening for both treatment groups (oral: 79.3 versus 54.1; IV: 84.4 versus 51.0; p < 0.001 for both. Most patients reported improvement in GI symptom severity and frequency from baseline at all post-screening assessments (>90% at Month 10. In the CURRENT subanalysis >60% of patients reported improvements in heartburn or acid reflux and >70% indicated improvement in other stomach upset at month 6. Postmenopausal women with GI irritability with daily or weekly BPs experienced improvement in symptoms with extended dosing monthly or quarterly ibandronate compared with baseline.Keywords: ibandronate, osteoporosis, bisphosphonate, gastrointestinal

  1. Development of a new rapid HPLC method for the fractionation of histones

    International Nuclear Information System (INIS)

    Gurley, L.R.; Valdez, J.G.; Prentice, D.A.; Spall, W.D.

    1983-01-01

    To study histone functions, it is necessary to fractionate the histones into their five classes (H1, H2A, H2B, H3 and H4) and then to subfractionate these classes into variants having slightly different primary structures and into different phosphorylated and acetylated forms. With the advent of high-performance liquid chromatography (HPLC), it was hoped that laborious and time-consuming conventional methods could be replaced by a simple, rapid, high-resolving HPLC method for fractionating histones. However, problems of irreversible adsorption of the histones to HPLC column packings discouraged this development. Our laboratory has now determined that the strong adsorption of histones to HPLC columns results from two different forces: (1) polar interactions between the histones and the silanol groups of silica-based HPLC column packing, and (2) hydrophobic interactions between the histones and the bound organic phase of the column packings. By minimizing these forces, we have succeeded in developing an HPLC method suitable for histone studies

  2. Bilateral orbital infarction and retinal detachment in a previously undiagnosed sickle cell hemoglobinopathy African child

    Science.gov (United States)

    Helen, Onakpoya Oluwatoyin; Ajite, K. O.; Oyelami, O. A.; Asaleye, C. M.; Adeoye, A. O.

    2013-01-01

    Bone infarction involving the orbit in sickle cell disease is not common. Bilateral orbital infarction in a previously undiagnosed sickle cell hemoglobinopathy has not been previously reported. In this report, we present a case of an 11-year-old previously undiagnosed sickle cell disease Nigerian girl with severe acute bilateral orbital infarction and retinal detachment to highlight that hemoglobinopathy induced orbital infarction should be considered in African children with acute onset proptosis with or without previous history of sickle cell hemoglobinopathy. PMID:23901183

  3. RP-HPLC Analysis of Quercetin in the Extract of Sambong (Blumea balsamifera (L DC Leaves

    Directory of Open Access Journals (Sweden)

    Joanna V. Toralba

    2015-06-01

    Full Text Available Blumea balsamifera (L DC, known in the Philippines as sambong, is an herb valued for its health benef its especially in the management of urolithiasis. Various phytochemicals, including flavonoids such as quercetin, have been determined in sambong leaves. A reversed-phase high-performance liquid chromatographic method (RP-HPLC was developed for the quantitative determination of quercetin in the methanol extract of sambong leaves obtained from Leyte, Cotabato, and Nueva Ecija, Philippines. The methanol extracts of sambong were prepared by maceration followed by rotary evaporation. The solid phase extraction (SPE for the sample cleanup involved the use of a C18 SPE packing, a 0.5-mL sample load (50 mg/mL solution, and elution with 4-mL of 80:20 Methanol:0.5% H3PO4. The HPLC conditions for the determination of quercetin involved the use of a C18 4.6-mm x 250-mm column maintained at 30°C, 254-nm UV detection, and a mobile phase composition of 25 parts methanol and 75 parts mixture of 0.5% H3PO4 and 0.2% triethylamine with a 1 mL/min flow rate in gradient elution. A good linearity at the concentration range of 3.72–124 μg/mL of quercetin standard (r2=0.9989 was observed with the limits of detection (LOD and quantitation (LOQ at 0.68 ng/mL and 2.28 ng/mL, respectively. The intra-day (n=5- and inter-day (n=3 precision values were satisfactory (%RSD <2%. The recovery eff iciency of the SPE sample cleanup step, which was checked by spiking sambong solution with quercetin standard, was 102.41%. The quercetin contents are 0.2337mg, 0.1350mg, and 0.2940mg per gram of the powdered dried leaves of sambong from Nueva Ecija, Cotabato, and Leyte, respectively. This is the f irst report of quercetin content in the leaves of sambong collected from the Philippines.

  4. NMR, HS-SPME-GC/MS, and HPLC/MSn Analyses of Phytoconstituents and Aroma Profile of Rosmarinus eriocalyx.

    Science.gov (United States)

    Bendif, Hamdi; Miara, Mohamed Djamel; Peron, Gregorio; Sut, Stefania; Dall'Acqua, Stefano; Flamini, Guido; Maggi, Filippo

    2017-10-01

    In this work, a comprehensive study on the chemical constituents of the aerial parts of Rosmarinus eriocalyx (Lamiaceae), an aromatic shrub traditionally consumed as a food and herbal remedy in Algeria, is presented. The aroma profile was analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC/MS), whereas the crude extract constituents were analyzed by 1 H-NMR and by high performance liquid chromatography coupled with mass spectrometry (HPLC/MS n ). Thirty-nine volatile compounds, most of them being monoterpenes, have been identified, with camphor, camphene, and α-pinene as the most abundant constituents. 1 H-NMR analysis revealed the presence of phenolic compounds and betulinic acid while HPLC/MS n allowed the identification of glycosilated and aglyconic flavonoids as well as phenylpropanoid derivatives. Some of these constituents, namely as betulinic acid, rosmanol, and cirsimaritin were reported for the first time in R. eriocalyx. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

  5. Qualitative and quantitative determination of yohimbine in authentic yohimbe bark and in commercial aphrodisiacs by HPLC-UV-API/ MS methods.

    Science.gov (United States)

    Zanolari, Boris; Ndjoko, Karine; Ioset, Jean-Robert; Marston, Andrew; Hostettmann, Kurt

    2003-01-01

    The development and validation of a rapid qualitative and quantitative method based on an HPLC-UV-MS technique with atmospheric pressure chemical ionisation and electrospray ionisation for the analysis of yohimbine in a number of commercial aphrodisiac products is reported. HPLC with multiple-stage mass spectrometry experiments allowed the identification of the target compound and increased the selectivity of complex analyses such as those involved with multi-botanical preparations. The precision and the robustness of the method were improved by the use of two internal standards: codeine for UV detection and deuterium-labelled yohimbine for MS detection. Twenty commercial aphrodisiac preparations were analysed and the amount of yohimbine measured and expressed as the maximal dose per day suggested on product labels ranged from 1.32 to 23.16 mg.

  6. Identification and quantification of flavonoids and chromes in Baeckea frutescens by using HPLC coupled with diode-array detection and quadruple time-of-flight mass spectrometry.

    Science.gov (United States)

    Jia, Bei-Xi; Huangfu, Qian-Qian; Ren, Feng-Xiao; Jia, Lu; Zhang, Yan-Bing; Liu, Hong-Min; Yang, Jie; Wang, Qiang

    2015-01-01

    This article marks the first report on high-performance liquid chromatography (HPLC) coupled with diode-array detection (DAD) and quadruple time-of-flight mass spectrometry (Q-TOF/MS) for the identification and quantification of main bioactive constituents in Baeckea frutescens. In total, 24 compounds were identified or tentatively characterised based on their retention behaviours, UV profiles and MS fragment information. Furthermore, a validated method with good linearity, sensitivity, precision, stability, repeatability and accuracy was successfully applied for simultaneous determination of five flavonoids and one chromone in different plant parts of B. frutescens collected at different harvest times, and their dynamic contents revealed the appropriate harvest times. The established HPLC-DAD-Q-TOF/MS using multi-bioactive markers was proved to be a validated strategy for the quality evaluation on both raw materials and related products of B. frutescens.

  7. Carotenoid composition of jackfruit (Artocarpus heterophyllus), determined by HPLC-PDA-MS/MS.

    Science.gov (United States)

    de Faria, A F; de Rosso, V V; Mercadante, A Z

    2009-06-01

    Carotenoids are pigments responsible for the yellow-reddish color of many foods and are related to important functions and physiological actions, preventing several chronic-degenerative diseases. The objective of this study was to confirm the carotenoid composition of jackfruit by high-performance liquid chromatography connected to photodiode array and mass spectrometry detectors (HPLC-PDA-MS/MS). The main carotenoids were all-trans-lutein (24-44%), all-trans-beta-carotene (24-30%), all-trans-neoxanthin (4-19%), 9-cis-neoxanthin (4-9%) and 9-cis-violaxanthin (4-10%). Either qualitative or quantitative differences, mainly related to the lutein proportion, were found among three batches of jackfruit. Since the fruits from batch A showed significantly lower contents for almost all carotenoids, it also had the lowest total carotenoid content (34.1 microg/100 g) and provitamin A value, whereas the total carotenoid ranged from 129.0 to 150.3 microg/100 g in the other batches. The provitamin A values from batches B and C were 3.3 and 4.3 microg RAE/100 g, respectively. The carotenoid composition of jackfruit was successfully determined, where 14 of the 18 identified carotenoids were reported for first time. Differences among batches may be due to genetic and/or agricultural factors.

  8. Clinical applications of HPLC-competitive protein binding assay for serum 25-hydroxyvitamin D

    International Nuclear Information System (INIS)

    Yang Shouli

    1989-01-01

    This report describes the clinical applications of HPLC-competitive protein binding assay for serum 25(OH) Vit D in 156 cases. Serum 25(OH) Vit D of normal human was 33.1 +- 14.8 nmol/L (13.2 +- 5.9 ng/ml), while for various diseases are as follows: rickets, 18.0 +- 9.0 nmol/L (7.2 +- 3.6 ng/ml, n = 36, P 0.1); pneumonia of children, 33.8 +- 14.8 nmol/L (13.5 +- 5.9 ng/ml, n = 10, P > 0.5); cirrhosis, 13.8 +- 11.3 nmol/L (5.5 +- 4.5 ng/ml, n = 9, P 0.2); administration of anticonvulsant (1 to 15 years), 19.0 +- 6.5 nmol/L (7.6 +- 2.6 ng/ml, n = 19, P 6 months), 15.3 +- 5.0 nmol/L (6.1 +- 2.0 ng/ml, n = 6, P 0.5); pregnant women, 39.8 +- 16.5 nmol/L (15.9 +- 6.6 ng/ml, n = 7, P > 0.1). We found it is a useful reference value for most of the above diseased state especially for differentiation between rickets and hypervitaminosis

  9. Isolation of {sup 163}Ho from dysprosium target material by HPLC for neutrino mass measurements

    Energy Technology Data Exchange (ETDEWEB)

    Mocko, Veronika; Taylor, Wayne A.; Nortier, Francois M.; Engle, Jonathan W.; Pollington, Anthony D.; Kunde, Gerd J.; Rabin, Michael W.; Birnbaum, Eva R. [Los Alamos National Laboratory, Los Alamos, NM (United States). Chemistry Div.; Barnhart, Todd E.; Nickles, Robert J. [Univ. Wisconsinn, Madison, WI (United States). Dept. of Medical Physics

    2015-07-01

    The rare earth isotope {sup 163}Ho is of interest for neutrino mass measurements. This report describes the isolation of {sup 163}Ho from a proton-irradiated dysprosium target and its purification. A Dy metal target was irradiated with 16 MeV protons for 10 h. After target dissolution, {sup 163}Ho was separated from the bulk Dy via cation-exchange high performance liquid chromatography using 70 mmol dm{sup -3} α-hydroxyisobutyric acid as the mobile phase. Subsequent purification of the collected Ho fraction was performed to remove the α-hydroxyisobutyrate chelating agent and to concentrate the Ho in a low ionic strength aqueous matrix. The final solution was characterized by MC-ICP-MS to determine the {sup 163}Ho/{sup 165}Ho ratio, {sup 163}Ho and the residual Dy content. The HPLC purification process resulted in a decontamination factor 1.4 x 10{sup 5} for Dy. The isolated Ho fraction contained 24.8 ± 1.3 ng of {sup 163}Ho corresponding to holmium recovery of 72 ± 3%.

  10. HPLC mapping of second generation ethanol production with lignocelluloses wastes and diluted sulfuric hydrolysis

    Directory of Open Access Journals (Sweden)

    Diogo José Horst

    2014-09-01

    Full Text Available Wood wastes are potential material for second generation ethanol production within the concept of residual forest bio-refinery. Current paper reports on ethanol production employing an HPLC method for monitoring the chemical content dispersed in the hydrolysate liquor after fermented. The proton-exchange technique was the analytical method employed. Twelve types of wood chips were used as biomass, including Hymenolobium petraeum, Tabebuia cassinoides, Myroxylon peruiferum, Nectandra lanceolata, Ocotea catharinensis, Cedrelinga catenaeformis, Cedrela fissilis Vell, Ocotea porosa, Laurus nobilis, Balfourodendron riedelianum, Pinus Elliotti and Brosimum spp. The influence of diluted sulfuric hydrolysis on the yeast Saccharomyces cerevisiae during the fermentation assay was also investigated. Standard compounds mapped in the analysis comprised fructose, lactic acid, acetic acid, glycerol, glucose and ethanol. The yeast showed ethanol productivity between 0.75 and 1.91 g L-1 h-1, respectively, without the addition of supplementary nutrients or detoxification. The use of these materials for the bioconversion of cellulose into ethanol has been proved. Current analysis contributes towards the production of biofuels by wastes recovery and by process monitoring and optimization.

  11. Determination of ortho-tyrosine in irradiated protein containing foods by HPLC

    International Nuclear Information System (INIS)

    Mischke, J.; Voehringer, M.; Helle, N.; Boegl K.W.; Schreiber, G.A.

    1993-01-01

    In order to control the processing and trading of irradiated foodstuffs several chemical and physical methods have been developed to identify irradiation induced changes. The three most promising methods are gas chromatorgraphic determination of radiation induced volatiles from the lipid content of foods, thermoluminescence measurements on minerals and e.s.r.-spectroscopic measurements on solids and food contents with a low water amount. There is a lack in detecting the irradiation in foods with a high protein content. It is based on the radiation induced hydroxylation of phenylalanine, forming small amounts of ortho- (and meta-) tyrosine. This method can be useful for foods with a low lipid content such as shrimps and pure egg-white. The results obtained on shrimps and egg-white are promising. All shrimp samples showed a good dose dependence which was similar to results reported by Chuaqui-Offermanns and McDougall obtained on frozen materials (chicken) irradiated at a slightly higher dose rate. There are not enough data about o-tyrosine-contents in different kinds of unirradiated shrimps. Therfore next step will be the analysis of a great number of various samples. With these information and by the use of an internal standard it should be possible to apply the HPLC method for routine analysis. As internal standards α-methyltyrosine or 4-hydroxyphenylglycine could be used. (orig./vhe)

  12. HPLC studies of aquatic humic compounds and complexes from the Drigg Research Site, Cumbria

    International Nuclear Information System (INIS)

    Smith, B.

    1991-01-01

    This report describes an investigation into the applicability of high performance liquid chromatographic techniques for the separation of the complex mixtures of organic acids commonly found in groundwaters. This work has shown that reverse phase ion-pair chromatography using a large pore stationary phase can be successfully applied to humic material in both natural and concentrated groundwater from the Drigg Research Site. The methodology separates the organic species into a number of well resolved components the majority of which have a molecular weight of greater than 500 Dalton. Separations obtained have been qualitatively and quantitatively analysed using a Diode array spectrophotometer. The components in excess of 500 Dalton show UV absorption spectra similar to humic and fulvic acids where as the component with a molecular weight of less than 500 Dalton shows a sharp UV absorption cutoff at 230 nm. It was noted that this component was not removed by passage through DEAEA cellulose. Reverse phase HPLC was also investigated, and results were found to be consistent with a separation based on an ion-repulsion/size exclusion mechanism. It was concluded that any separation based on this mechanism is likely to suffer from poor inter run reproducibility and must therefore be discounted as a suitable method. Similarly, ion-suppression reverse phase was shown to be equally impracticable, requiring a mobile phase pH of less than 2 to obtain separation (this low pH renders a silica based stationary phase unstable). (author)

  13. Analysis of alcohol dehydrogenase inhibitors from Desmodium styracifolium using centrifugal ultrafiltration coupled with HPLC-MS

    Directory of Open Access Journals (Sweden)

    Liu Liangliang

    2015-01-01

    Full Text Available Alcohol dehydrogenase (ADH inhibitors play an important role in the treatment of human methanol or ethylene glycol poisoning and the suppression of acetaldehyde accumulation in alcoholics. In this study, centrifugal ultrafiltration coupled with high performance liquid chromatography-mass spectrometry (HPLC-MS was utilized to screen and identify ADH inhibitors from ethyl acetate extract of Desmosium styracifolium (Osb. Merr. The experiment conditions of centrifugal ultrafiltration were optimized. At the optimum conditions (ADH concentration: 37.5 μg mL-1, incubation time: 90 min, pH: 7.0 and temperature: 15°C, formononetin and aromadendrin were successfully screened and identified from ethyl acetate extract of Desmodium styracifolium. The screening result was verified by ADH inhibition assays. The IC50 values of formononetin and aromadendrin were 70.8 and 84.7 μg mL-1, which were accorded with the binding degrees of them. Aromadendrin was first reported to have inhibitory activity on ADH. This method provided an effective way to screen active compounds from natural products.

  14. Stability-Indicating RP-HPLC Method for Assay of Silver Lactate

    Directory of Open Access Journals (Sweden)

    V. Srinivasan

    2011-01-01

    Full Text Available A simple, economic and time-efficient stability-indicating, reverse-phase high-performance liquid chromatographic (RP-HPLC method has been developed for analysis of silver lactate in the presence of degradation products generated by decomposition. When silver lactate was subjected to acid hydrolysis, base hydrolysis, oxidative, photolytic, humidity and thermal stress, degradation was observed during base hydrolysis, oxidation, humidity and thermal stress. The drug was found to be stable to other stress conditions. Successful chromatographic condition of the drug from the degradation products formed under stress conditions was achieved on a phenomenex Gemini column with potassium dihydrogen phosphate buffer, pH adjusted to 2.2 with orthophosphoric acid, as mobile phase. The method was validated for linearity, precision, specificity and robustness and can be used for quality-control during manufacture and assessment of the stability of samples of silver lactate. To the best of our knowledge, a validated stability-indicating LC assay method for silver lactate based on lactic acid is reported for the first time.

  15. Arsenic-containing fatty acids and hydrocarbons in marine oils - Determination using reversed-phase HPLC-ICP-MS and HPLC-qTOF-MS

    DEFF Research Database (Denmark)

    Sele, Veronika; Sloth, Jens Jørgen; Holmelid, Bjarte

    2014-01-01

    ; dimethylarsinate (DMA), triphenylarsinoxide (Ph3AsO) and a synthesized arsenic-containing hydrocarbon (AsHC) (dimethylarsinoyl nonadecane; C21H43AsO). The observed variation in signal intensity for arsenic during the gradient elution profile in reversed-phase HPLC was compensated for by determining the time...

  16. Impact of previously disadvantaged land-users on sustainable ...

    African Journals Online (AJOL)

    Impact of previously disadvantaged land-users on sustainable agricultural ... about previously disadvantaged land users involved in communal farming systems ... of input, capital, marketing, information and land use planning, with effect on ...

  17. HPLC analysis of vitamin B6 in foods

    Directory of Open Access Journals (Sweden)

    V.-M. OLLILAINEN

    2008-12-01

    Full Text Available The objective of this work was to evaluate the methods for determination of vitamin B6 in foods. To achieve this, the literature review focused on sample treatment and liquid chromatographic analysis of vitamin B6 related compounds. In the experimental part, the chosen sample pretreatment and the high-performance liquid chromatographic (HPLC method were validated, and used to produce vitamin B6 data on various food items commonly consumed in Finland. The main emphasis of the sample treatment was on the extraction efficiency and the maintenance of the original concentration profile of the vitamers. Several acid extraction procedures were tested for this purpose. Perchloric acid was chosen as the extraction agent. Routine food analysis was then performed using dilute ice-cold perchloric acid extraction followed by an internally standardized ion-paired reversed-phase liquid chromatography. Food samples were hydrolyzed with takadiastase and alkaline phosphatase enzymes, phosphorylated and glycosylated vitamers were quantitated before and after the enzymatic digestion. This procedure enabled the extraction of vitamin B6 compounds in their intact forms, and the measurement of free, phosphorylated and glycosylated forms. The maintenance of the concentration profile of the vitamers was verified by using 14C -labeled pyridoxal 5'-phosphate in the examination of the extraction procedure. The extraction efficiency and laboratory performance were confirmed by interlaboratory studies. Up-to-date data on vitamin B6 content of about fifty common food items was produced. The data includes the results from meat and poultry, fish and fish product, dairy product, cereal and vegetable, and ready-to-eat food samples. Free and phosphorylated vitamin B6 compounds were measured in all food groups, and the glycosylated vitamer fraction was analyzed in all plant-derived foods. The results obtained in this work showed that vitamin B6 content of nearly all foods of plant

  18. 22 CFR 40.91 - Certain aliens previously removed.

    Science.gov (United States)

    2010-04-01

    ... 22 Foreign Relations 1 2010-04-01 2010-04-01 false Certain aliens previously removed. 40.91... IMMIGRANTS UNDER THE IMMIGRATION AND NATIONALITY ACT, AS AMENDED Aliens Previously Removed § 40.91 Certain aliens previously removed. (a) 5-year bar. An alien who has been found inadmissible, whether as a result...

  19. Cluster analysis of historical and modern hard red spring wheat cultivars based on parentage and HPLC analysis of gluten forming proteins

    Science.gov (United States)

    In this study, 30 hard red spring (HRS) wheat cultivars released between 1910 and 2013 were analyzed to determine how they cluster in terms of parentage and protein data, analyzed by reverse-phase HPLC (RP-HPLC) of gliadins, and size-exclusion HPLC (SE-HPLC) of unreduced proteins. Dwarfing genes in...

  20. Determining root correspondence between previously and newly detected objects

    Science.gov (United States)

    Paglieroni, David W.; Beer, N Reginald

    2014-06-17

    A system that applies attribute and topology based change detection to networks of objects that were detected on previous scans of a structure, roadway, or area of interest. The attributes capture properties or characteristics of the previously detected objects, such as location, time of detection, size, elongation, orientation, etc. The topology of the network of previously detected objects is maintained in a constellation database that stores attributes of previously detected objects and implicitly captures the geometrical structure of the network. A change detection system detects change by comparing the attributes and topology of new objects detected on the latest scan to the constellation database of previously detected objects.

  1. Sugar Composition Analysis of Fuzi Polysaccharides by HPLC-MSn and Their Protective Effects on Schwann Cells Exposed to High Glucose

    Directory of Open Access Journals (Sweden)

    Bei-Bei Wang

    2016-11-01

    Full Text Available Fuzi has been used to treat diabetic complications for many years in china. In a previous study, we have shown that Fuzi aqueous extract can attenuate Diabetic peripheral neuropathy (DPN in rats and protect Schwann cells from injury. Thus, the protective effect of Fuzi polysaccharides (FPS on high glucose-induced SCs and the preliminary mechanism were investigated. Firstly, the FPS were obtained and their monose composition was analyzed by the combination of pre-column derivatization and high performance liquid chromatography coupled with electrospray ionization multi-tandem mass spectrometry (HPLC/ESI-MSn. The results witnessed the efficiency of this method and seven monosaccharides were tentatively identified, among which fucose was first reported. Simultaneously, m/z 215 can be considered as diagnostic ions to confirm the number of monosaccharides. Next, high glucose-induced SC model was applied and divided into model group, treated group of FPS, normal and osmotic control group. After treatment for 48 h, the data showed FPS could significantly decrease the intracellular ROS and apoptosis, which were determined by the corresponding fluorescent probes. Then, the expression of oxidative stress-related proteins in SCs were measured by Western blot. Furthermore, the protein tests found that FPS markedly up-regulated superoxide dismutase (SOD, catalase (CAT and peroxisome proliferator-activated receptor gamma coactivator 1-alpha (PGC-1α protein level, but down-regulated NADPH oxidase-1 (Nox1 protein level. Moreover, FPS could also increase AMP-activated protein kinase (AMPK activation significantly. Hence, we preliminary deduced that AMPK-PGC-1α pathway may play an important role in the protective effect of FPS against high glucose-induced cell damage.

  2. Radon anomalies prior to earthquakes (1). Review of previous studies

    International Nuclear Information System (INIS)

    Ishikawa, Tetsuo; Tokonami, Shinji; Yasuoka, Yumi; Shinogi, Masaki; Nagahama, Hiroyuki; Omori, Yasutaka; Kawada, Yusuke

    2008-01-01

    The relationship between radon anomalies and earthquakes has been studied for more than 30 years. However, most of the studies dealt with radon in soil gas or in groundwater. Before the 1995 Hyogoken-Nanbu earthquake, an anomalous increase of atmospheric radon was observed at Kobe Pharmaceutical University. The increase was well fitted with a mathematical model related to earthquake fault dynamics. This paper reports the significance of this observation, reviewing previous studies on radon anomaly before earthquakes. Groundwater/soil radon measurements for earthquake prediction began in 1970's in Japan as well as foreign countries. One of the most famous studies in Japan is groundwater radon anomaly before the 1978 Izu-Oshima-kinkai earthquake. We have recognized the significance of radon in earthquake prediction research, but recently its limitation was also pointed out. Some researchers are looking for a better indicator for precursors; simultaneous measurements of radon and other gases are new trials in recent studies. Contrary to soil/groundwater radon, we have not paid much attention to atmospheric radon before earthquakes. However, it might be possible to detect precursors in atmospheric radon before a large earthquake. In the next issues, we will discuss the details of the anomalous atmospheric radon data observed before the Hyogoken-Nanbu earthquake. (author)

  3. Combined HPLC-CUPRAC (cupric ion reducing antioxidant capacity) assay of parsley, celery leaves, and nettle.

    Science.gov (United States)

    Yildiz, Leyla; Başkan, Kevser Sözgen; Tütem, Esma; Apak, Reşat

    2008-10-19

    This study aims to identify the essential antioxidant compounds present in parsley (Petroselinum sativum) and celery (Apium graveolens) leaves belonging to the Umbelliferae (Apiaceae) family, and in stinging nettle (Urtica dioica) belonging to Urticaceae family, to measure the total antioxidant capacity (TAC) of these compounds with CUPRAC (cupric ion reducing antioxidant capacity) and ABTS spectrophotometric methods, and to correlate the TAC with high performance liquid chromatography (HPLC) findings. The CUPRAC spectrophotometric method of TAC assay using copper(II)-neocuproine (2,9-dimethyl-1,10-phenanthroline) as the chromogenic oxidant was developed in our laboratories. The individual antioxidant constituents of plant extracts were identified and quantified by HPLC on a C18 column using a modified mobile phase of gradient elution comprised of MeOH-0.2% o-phosphoric acid and UV detection for polyphenols at 280 nm. The TAC values of HPLC-quantified antioxidant constituents were found, and compared for the first time with those found by CUPRAC. The TAC of HPLC-quantified compounds accounted for a relatively high percentage of the observed CUPRAC capacities of plant extracts, namely 81% of nettle, 60-77% of parsley (in different hydrolyzates of extract and solid sample), and 41-57% of celery leaves (in different hydrolyzates). The CUPRAC total capacities of the 70% MeOH extracts of studied plants (in the units of mmol trolox g(-1)plant) were in the order: celery leaves>nettle>parsley. The TAC calculated with the aid of HPLC-spectrophotometry did not compensate for 100% of the CUPRAC total capacities, because all flavonoid glycosides subjected to hydrolysis were either not detectable with HPLC, or not converted to the corresponding aglycons (i.e., easily detectable and quantifiable with HPLC) during the hydrolysis step.

  4. 77 FR 44113 - Airworthiness Directives; Gulfstream Aerospace LP (Type Certificate Previously Held by Israel...

    Science.gov (United States)

    2012-07-27

    ... Airworthiness Directives; Gulfstream Aerospace LP (Type Certificate Previously Held by Israel Aircraft... Aerospace LP (Type Certificate previously held by Israel Aircraft Industries, Ltd.) Model Gulfstream G150... to the manufacturer. This action was prompted by a report from the Civil Aviation Authority of Israel...

  5. VERIFICATION HPLC METHOD OF QUANTITATIVE DETERMINATION OF AMLODIPINE IN TABLETS

    Directory of Open Access Journals (Sweden)

    Khanin V. A

    2014-10-01

    a volume of 100.0 ml. Preparation of the working standard solution sample amlodipine besylate. 50.0 mg of amlodipine RCC dissolved in methanol and dilute with the same solvent to 50.0 ml. 5.0 ml of this solution argue with methanol to volume 100.0 ml. Before the major controlled trials validated the existence of documents certifying the suitability vykorystovanoho equipment, raw materials and chemicals. Validation of the methodology was carried out in accordance with the requirements of SPhU. Results & discussion. Linearity methods defined within 80-120% of nominal concentrations. The linearity of the methods supported by the entire range of concentrations studied (b=0.9845, Sb=0,01473, a=1.5282, Sa=1.4956, S0=0.5486, r=0.9992. It is proved that the validated method characterized by sufficient convergence and accuracy over the entire range of concentrations (ΔZ=1.03, δ%=0.09. Conclusion. During verification methods of quantitative determination of amlodipine besylate tablets were studied characteristics validated HPLC method: accuracy, linearity, precision, specificity, and internal laboratory precision. Validation technique characteristics do not exceed the critical value of error (1.6% and characterized by qualitative analytical indicators. This technique can be correctly reproduced in the laboratory conditions, and is independent of the excipients.

  6. Simultaneous detection of water-soluble vitamins using the High Performance Liquid Chromatography (HPLC - a review

    Directory of Open Access Journals (Sweden)

    Rosemond Godbless Dadzie

    2014-01-01

    Full Text Available The water-soluble vitamins (WSV: ascorbic acid (vitamin C, thiamine (B1, riboflavin (B2, niacin (B3, panthothenic acid (B5, pyridoxine, and pyridoxal (B6, folic acid (B9, biotin(B8 , and B12 are very essential in the diet of humankind. As a result of ever increasing pressures from both consumers and legal enforcers, to specify accurately nutritive compositions of WSV that are present in food materials, many researchers have attempted to fill this niche through the provision of highly sensitive and rapid high performance liquid chromatography (HPLC procedures. In view of the health benefits of WSV, a replete of HPLC methods have been developed for simultaneous determination of their contents in nature and fortified food samples, nutritional supplements, as well as blood plasmas. The rate of losses of these vitamins during food processing and analysis, in addition to their transient dynamics, presents complexities in developing a highly sensitive HPLC procedure for their simultaneous separations and assays. This review critically assesses the different HPLC procedures developed by researchers and available in the open literature for simultaneous determination of water-soluble vitamins (WSV in dried tropical fruits materials. The study revealed that not a single chromatographic run developed by researchers can simultaneously elute all the WSV at a time. However, the HPLC procedures that are capable of determining all the WSV were coupled with electrospray ionization mass spectroscopy (ESI-MS, thus making the set-up expensive.

  7. Comparison of transferrin isoform analysis by capillary electrophoresis and HPLC for screening congenital disorders of glycosylation.

    Science.gov (United States)

    Dave, Mihika B; Dherai, Alpa J; Udani, Vrajesh P; Hegde, Anaita U; Desai, Neelu A; Ashavaid, Tester F

    2018-01-01

    Transferrin, a major glycoprotein has different isoforms depending on the number of sialic acid residues present on its oligosaccharide chain. Genetic variants of transferrin as well as the primary (CDG) & secondary glycosylation defects lead to an altered transferrin pattern. Isoform analysis methods are based on charge/mass variations. We aimed to compare the performance of commercially available capillary electrophoresis CDT kit for diagnosing congenital disorders of glycosylation with our in-house optimized HPLC method for transferrin isoform analysis. The isoform pattern of 30 healthy controls & 50 CDG-suspected patients was determined by CE using a Carbohydrate-Deficient Transferrin kit. The results were compared with in-house HPLC-based assay for transferrin isoforms. Transferrin isoform pattern for healthy individuals showed a predominant tetrasialo transferrin fraction followed by pentasialo, trisialo, and disialotransferrin. Two of 50 CDG-suspected patients showed the presence of asialylated isoforms. The results were comparable with isoform pattern obtained by HPLC. The commercial controls showed a <20% CV for each isoform. Bland Altman plot showed the difference plot to be within +1.96 with no systemic bias in the test results by HPLC & CE. The CE method is rapid, reproducible and comparable with HPLC and can be used for screening Glycosylation defects. © 2017 Wiley Periodicals, Inc.

  8. An industry consensus study on an HPLC fluorescence method for the determination of (±)-catechin and (±)-epicatechin in cocoa and chocolate products.

    Science.gov (United States)

    Shumow, Laura; Bodor, Alison

    2011-07-05

    This manuscript describes the results of an HPLC study for the determination of the flavan-3-ol monomers, (±)-catechin and (±)-epicatechin, in cocoa and plain dark and milk chocolate products. The study was performed under the auspices of the National Confectioners Association (NCA) and involved the analysis of a series of samples by laboratories of five member companies using a common method. The method reported in this paper uses reversed phase HPLC with fluorescence detection to analyze (±)-epicatechin and (±)-catechin extracted with an acidic solvent from defatted cocoa and chocolate. In addition to a variety of cocoa and chocolate products, the sample set included a blind duplicate used to assess method reproducibility. All data were subjected to statistical analysis with outliers eliminated from the data set. The percent coefficient of variation (%CV) of the sample set ranged from approximately 7 to 15%. Further experimental details are described in the body of the manuscript and the results indicate the method is suitable for the determination of (±)-catechin and (±)-epicatechin in cocoa and chocolate products and represents the first collaborative study of this HPLC method for these compounds in these matrices.

  9. Development and Validation of a HPLC-UV Method for Extraction Optimization and Biological Evaluation of Hot-Water and Ethanolic Extracts of Dendropanax morbifera Leaves

    Directory of Open Access Journals (Sweden)

    Hyung-Jae Choi

    2018-03-01

    Full Text Available Dendropanax morbifera Leveille (Araliaceae has been used in traditional oriental remedies for cancer, inflammation, diabetes, and thrombosis. However, a validated analytical method, standardization, and optimization of extraction conditions with respect to biological activity have not been reported. In this study, a simple and validated HPLC method for identifying and quantifying active substances in D. morbifera was developed. Hot water and ethanolic D. morbifera leaf extracts from different production regions were prepared and evaluated with regard to their chemical compositions and biological activities. The contents of active compounds such as rutin and chlorogenic acid were determined in four samples collected from different regions. The 80% ethanolic extract showed the best antioxidant activity, phenolic content, reducing power, and xanthine oxidase (XO inhibitory activity. The validated HPLC method confirmed the presence of chlorogenic acid and rutin in D. morbifera leaf extracts. The antioxidant and XO inhibitory activity of D. morbifera extract could be attributed to the marker compounds. Collectively, these results suggest that D. morbifera leaves could be beneficial for the treatment or prevention of hyperuricemia-related disease, and the validated HPLC method could be a useful tool for the quality control of food or drug formulations containing D. morbifera.

  10. Tandem solid-phase extraction followed by HPLC-ESI/QTOF/MS/MS for rapid screening and structural identification of trace diterpenoids in flowers of Rhododendron molle.

    Science.gov (United States)

    Zou, Hong-Yan; Luo, Jun; Xu, De-Ran; Kong, Ling-Yi

    2014-01-01

    'Naoyanghua', composed of the flowers of Rhododendron molle G. Don, is a traditional Chinese medicine that is widely known for its toxicity. Grayanane-type diterpenoids are the main active ingredients in R. molle, as well as possibly their toxicity: they are, however, difficult to isolate and analyse using common chromatographic methods, due to their small amounts and absence of conjugated groups, such as phenyl and α, β-unsaturated ketone. To establish a highly sensitive, selective and reliable method for the qualitative evaluation of trace diterpenoids in the flowers of R. molle by using tandem solid-phase extraction followed by high-performance liquid chromatography with electrospray ionisation quadrupole-time-of-flight mass spectrometry (HPLC-ESI/QTOF/MS/MS). Tandem solid phase extraction (SPE) was undertaken using a polyamide cartridge and a C18E cartridge in succession to enrich the trace diterpenoids. HPLC-ESI/QTOF/MS/MS was used to determine the fragmentation patterns of diterpenoids and to tentatively characterise their fragmentation pathways. HPLC-ESI/QTOF/MS/MS detected a total of 14 diterpenoids, eight of which were identified by comparison with literature sources and six based on fragmentation analysis. Among the latter six, rhodojaponin VI-3-glucoside was tentatively identified as a new diterpenoid glycoside and rhodojaponin VII, rhodojaponin IV and rhodojaponin I were reported from R. molle for the first time. By qualitative research of diterpenoids in this plant by HPLC-ESI/QTOF/MS/MS, a reliable methodology for the analysis of these active constituents of R. molle was established for the first time. Copyright © 2014 John Wiley & Sons, Ltd.

  11. Diversity oriented high-throughput screening of 1,3,4-oxadiazole modified chlorophenylureas and halogenobenzamides by HPLC with peptidomimetic calixarene-bonded stationary phases.

    Science.gov (United States)

    Bazylak, Grzegorz; Malak, Anna; Ali, Imran; Borowiak, Teresa; Dutkiewicz, Grzegorz

    2008-06-01

    Retention profiles in series of the neutral and highly hydrophobic 1,3,4-oxadiazoles containing chlorophenylurea and halogenobenzamide moiety and indicating analgesic activity were determined in the isocratic standard- and narrow-bore HPLC systems employing, respectively, various octadecylsilica and different calixarene bonded stationary phases. When acetonitrile - 2.65 mM phosphoric acid (55 : 45, %, v/v), pH* 3.25, mobile phase was applied retention of these compounds increased with decline of their overall hydrophobicity according to the general preference of more polar compounds by calixarene cavity in time of its non-specific host-guest supramolecular interactions with halogenated substances. The size of calixarene nanocavity and its upper-rim substitution did not change the observed retention order, resolution and selectivity of separation for oxadiazoles. Compared to the retention on the non-end-capped and the highly-end-capped octadecylsilica HPLC column a most improved separation of some regioisomers of halogenated 1,3,4-oxadiazoles were observed on both used calixarene-type HPLC supports. In addition, preliminary data on the self-assembled supramolecular crystal structure of exemplary 1,3,4-oxadiazolchlorophenylurea with cis-elongated conformation was reported and formation of the monovalent inclusion host-guest complexes between 1,3,4-oxadiazoles and each calixarene-type stationary phase was studied with molecular modelling MM+ and AM1 methods. The structural, isomeric and energetic factors leading to the hydrogen bond stabilized inclusion complexes between these species were considered and used for explanation of observed retention sequence and selectivity of 1,3,4-oxadiazoles separation in applied calixarene-based HPLC systems. All these data would be useful in future development of optimized procedures enabling encapsulation of 1,3,4-oxadiazolurea-type drugs with calixarenes.

  12. HPLC determination of chloride, bromide and iodide ions in drinking water and industrial effluents using trifluoromethylmercuric nitrate as derivatizing reagent

    International Nuclear Information System (INIS)

    Arain, M.A.; Bhanger, M.I.; Khuhawar, M.Y.

    1997-01-01

    A simple procedure for the simultaneous determination of various halides in drinking water and industrial effluents of Hyderabad and Iodized salt is reported. The method utilizes derivatization of halides through trifluoromethylmercuric nitrate in aqueous solution, extraction in petroleum ether followed by reverse phase HPLC separation using c-18 Lichrosorb column, 150 x 4 mm i.d., mobile phase methanol : water (20: 80) and UV detection at 225 nm. Linear calibration ranges for chloride, bromide and iodide (0-10 ug/mL) with correlation coefficient 0.996, 0.998 and 0.989 have been determined with lowest possible detection limit as 1.0, 0.25 and 1.5 Mu g/ml, respectively. The effect of various interfering ions is also discussed. (author)

  13. Rapid and Reliable HPLC Method for the Simultaneous Determination of Dihydroxyacetone, Methylglyoxal and 5-Hydroxymethylfurfural in Leptospermum Honeys.

    Directory of Open Access Journals (Sweden)

    Matthew Pappalardo

    Full Text Available A reliable determination of dihydroxyacetone, methylglyoxal and 5-hydroxymethylfurfural is essential to establishing the commercial value and antimicrobial potential of honeys derived from the Leptospermum species endemic to Australia and New Zealand. We report a robust method for quantitation of all three compounds in a single HPLC run. Honey samples (n = 6 that are derivatized with o-(2,3,4,5,6-Pentafluorobenzyl hydroxylamine were quantitated against a stable anisole internal standard. Linear regression analysis was performed using calibration standards for each compound (n = 6 and results indicated a high degree of accuracy (R2 = 0.999 for this method. The reliability of some commercial methylglyoxal solutions were found to be questionable. Effective quantitation of methylglyoxal content in honey is critical for researchers and industry, and the use of some commercial standards may bias data. Two accurate methylglyoxal standards are proposed, including a commercial standard and a derivative that can be prepared within the laboratory.

  14. 49 CFR 173.23 - Previously authorized packaging.

    Science.gov (United States)

    2010-10-01

    ... 49 Transportation 2 2010-10-01 2010-10-01 false Previously authorized packaging. 173.23 Section... REQUIREMENTS FOR SHIPMENTS AND PACKAGINGS Preparation of Hazardous Materials for Transportation § 173.23 Previously authorized packaging. (a) When the regulations specify a packaging with a specification marking...

  15. 28 CFR 10.5 - Incorporation of papers previously filed.

    Science.gov (United States)

    2010-07-01

    ... 28 Judicial Administration 1 2010-07-01 2010-07-01 false Incorporation of papers previously filed... CARRYING ON ACTIVITIES WITHIN THE UNITED STATES Registration Statement § 10.5 Incorporation of papers previously filed. Papers and documents already filed with the Attorney General pursuant to the said act and...

  16. 75 FR 76056 - FEDERAL REGISTER CITATION OF PREVIOUS ANNOUNCEMENT:

    Science.gov (United States)

    2010-12-07

    ... SECURITIES AND EXCHANGE COMMISSION Sunshine Act Meeting FEDERAL REGISTER CITATION OF PREVIOUS ANNOUNCEMENT: STATUS: Closed meeting. PLACE: 100 F Street, NE., Washington, DC. DATE AND TIME OF PREVIOUSLY ANNOUNCED MEETING: Thursday, December 9, 2010 at 2 p.m. CHANGE IN THE MEETING: Time change. The closed...

  17. Monitoring of monosaccharides, oligosaccharides, ethanol and glycerol during wort fermentation by biosensors, HPLC and spectrophotometry.

    Science.gov (United States)

    Monošík, Rastislav; Magdolen, Peter; Stredanský, Miroslav; Šturdík, Ernest

    2013-05-01

    The aim of the present study was to analyze sugar levels (namely maltose, maltotriose, glucose and fructose) and alcohols (ethanol and glycerol) during the fermentation process in wort samples by amperometric enzymatic biosensors developed by our research group for industrial application, HPLC and spectrophotometry, and to compare the suitability of the presented methods for determination of individual analytes. We can conclude that for the specific monitoring of maltose or maltotriose only the HPLC method was suitable. On the other hand, biosensors and spectrophotometry reflected a decrease in total sugar concentration better and were able to detect both glucose and fructose in the later stages of fermentation, while HPLC was not. This can be attributed to the low detection limits and good sensitivity of the proposed methods. For the ethanol and glycerol analysis all methods proved to be suitable. However, concerning the cost expenses and time analysis, biosensors represented the best option. Copyright © 2012 Elsevier Ltd. All rights reserved.

  18. ANALISIS RESIDU KLORPIRIFOS DALAM SAYUR-SAYURAN DENGAN TEKNIK HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC

    Directory of Open Access Journals (Sweden)

    Aman Sentosa Panggabean

    2016-06-01

    Full Text Available The research about analysis of chlorpyrifos residue in vegetables by using High Performance Liquid Chromatography (HPLC technique has been done. To obtain the optimal measurement results, the measurement performed several important parameters in the chromatographic system was composition of mobile phase, volume injection sample, flow rate and pH eluent. Optimum measurement conditions obtained was mobile phase composition (water : methanol with 70 : 30, volume injection sample are 5 mL, flow rate are 0.5mL/menit and pH eluent are 7. The analytical performance that obtained is good showed with the reproducibility value as percentage coefficient variance (% CV was 0.0664%, limit of detection (LOD was 0.44 ppm, with a recovery percentage of > 95%. The results obtained showed the HPLC technique can be used for the routine analysis in the determination of chlorpyrifos for the vegetable samples. Keywords: Chlorpyrifos, Vegetables, HPLC.

  19. Analysis of the extracts of Isatis tinctoria by new analytical approaches of HPLC, MS and NMR.

    Science.gov (United States)

    Zhou, Jue; Qu, Fan

    2011-01-01

    The methods of extraction, separation and analysis of alkaloids and indole glucosinolates (GLs) ofIsatis tinctoria were reviewed. Different analytical approaches such as High-pressure Liquid Chromatography (HPLC), Liquid Chromatography with Electrospray Ionization Mass Spectrometry (LC/ESI/MS), Electrospray Ionization Time-Of-Flight Mass Spectrometry (ESI-TOF-MS), and Nuclear Magnetic Resonance (NMR) were used to validate and identity of these constituents. These methods provide rapid separation, identification and quantitative measurements of alkaloids and GLs of Isatis tinctoria. By connection with different detectors to HPLC such as PDA, ELSD, ESI- and APCI-MS in positive and negative ion modes, complicated compounds could be detected with at least two independent detection modes. The molecular formula can be derived in a second step of ESI-TOF-MS data. But for some constituents, UV and MS cannot provide sufficient structure identification. After peak purification, NMR by semi-preparative HPLC can be used as a complementary method.

  20. Brief on -Hyphenated Methods of HPLC for Determining the Presence of Solutes.

    Directory of Open Access Journals (Sweden)

    Mohamad Taleuzzaman

    2017-02-01

    Full Text Available HPLC is the tool in liquid chromatography is unique because of particle size, smaller particle in the stationary phase, increase efficiency of a separation. However, if the particles are made smaller, capillary action increases and it becomes more difficult to drain the column under gravity. For quantitative analysis different types of detector is used in conjunction with HPLC which give precise and accurate result and it is apply according to the nature of the substance. Various types of detectors used in HPLC are mass spectrometry, infrared spectroscopy, visible spectroscopy, ultraviolet spectroscopy, fluorescence spectroscopy, nuclear magnetic resonance, conductivity measurement, and refractive index measurement. Each detector has its assets, limitations and sample types for which it is most effective. The recent development of the so-called hyphenated techniques has improved the ability to separate and identify multiple entities within a mixture.

  1. A uHPLC-MS mathematical modeling approach to dry powder inhaler single agglomerate analysis.

    Science.gov (United States)

    Pennington, Justin; Lena, John; Medendorp, Joseph; Ewing, Gary

    2011-10-01

    Demonstration of content uniformity (CU) is critical toward the successful development of dry powder inhalers (DPIs). Methods for unit dose CU determination for DPI products are well-established within the field of respiratory science. Recent advances in the area include a uHPLC-MS method for high-throughput uniformity analysis, which allows for a greater understanding of blending operations as the industry transitions to a quality-by-design approach to development. Further enhancements to this uHPLC-MS method now enable it to determine CU and sample weight at the single agglomerate level, which is roughly 50× smaller than a unit dose. When coupled with optical microscopy-based agglomerate sizing, the enhanced uHPLC-MS method can also predict the density and porosity of individual agglomerates. Expanding analytical capabilities to the single agglomerate level provides greater insights and confidence in the DPI manufacturing process.

  2. A novel HPLC method for separation of uranium from thorium using BEHSA modified semi preparative support

    International Nuclear Information System (INIS)

    Raju, Ch.Siva Kesava; Subramanian, M.S.; Sivaraman, N.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2006-01-01

    The determination of uranium and thorium is of great importance with respect to nuclear industry and environmental samples. High performance liquid chromatography (HPLC) has revolutionized as a powerful separation and analytical tool in the field of chemistry, biology, medicine, pharmacy, chemical technology, food science and many more. The major advantages of HPLC are its ability to provide rapid, high performance separations and extending the separations range from laboratory scale to preparative scale purification. HPLC became powerful technique for the separation of uranium and thorium. These methods were widely employed in applications such as separation of uranium from fission products and for the measurement of number of fissions as in the case of burn-up measurements on nuclear reactor fuels

  3. Validated Reverse Phase HPLC Method for the Determination of Impurities in Etoricoxib

    Directory of Open Access Journals (Sweden)

    S. Venugopal

    2011-01-01

    Full Text Available This paper describes the development of reverse phase HPLC method for etoricoxib in the presence of impurities and degradation products generated from the forced degradation studies. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation of etoricoxib was observed under base and oxidation environment. The drug was found stable in other stress conditions studied. Successful separation of the drug from the process related impurities and degradation products were achieved on zorbax SB CN (250 x 4.6 mm 5 μm particle size column using reverse phase HPLC method. The isocratic method employed with a mixture of buffer and acetonitrile in a ratio of 60:40 respectively. Disodium hydrogen orthophosphate (0.02 M is used as buffer and pH adjusted to 7.20 with 1 N sodium hydroxide solution. The HPLC method was developed and validated with respect to linearity, accuracy, precision, specificity and ruggedness.

  4. The integrated quality assessment of Chinese commercial dry red wine based on a method of online HPLC-DAD-CL combined with HPLC-ESI-MS.

    Science.gov (United States)

    Yu, Hai-Xiang; Sun, Li-Qiong; Qi, Jin

    2014-07-01

    To apply an integrated quality assessment strategy to investigate the quality of multiple Chinese commercial dry red wine samples. A comprehensive method was developed by combining a high performance liquid chromatography-diode array detector-chemiluminescence (HPLC-DAD-CL) online hyphenated system with an HPLC-ESI-MS technique. Chromatographic and H2O2-scavenging active fingerprints of thirteen batches of different, commercially available Chinese dry red wine samples were obtained and analyzed. Twenty-five compounds, including eighteen antioxidants were identified and evaluated. The dominant and characteristic antioxidants in the samples were identified. The relationships between antioxidant potency and the cultivated variety of grape, producing area, cellaring period, and trade mark are also discussed. The results provide the feasibility for an integrated quality assessment strategy to be efficiently and objectively used in quality (especially antioxidant activity) assessment and identification of dry red wine. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

  5. No discrimination against previous mates in a sexually cannibalistic spider

    Science.gov (United States)

    Fromhage, Lutz; Schneider, Jutta M.

    2005-09-01

    In several animal species, females discriminate against previous mates in subsequent mating decisions, increasing the potential for multiple paternity. In spiders, female choice may take the form of selective sexual cannibalism, which has been shown to bias paternity in favor of particular males. If cannibalistic attacks function to restrict a male's paternity, females may have little interest to remate with males having survived such an attack. We therefore studied the possibility of female discrimination against previous mates in sexually cannibalistic Argiope bruennichi, where females almost always attack their mate at the onset of copulation. We compared mating latency and copulation duration of males having experienced a previous copulation either with the same or with a different female, but found no evidence for discrimination against previous mates. However, males copulated significantly shorter when inserting into a used, compared to a previously unused, genital pore of the female.

  6. Implant breast reconstruction after salvage mastectomy in previously irradiated patients.

    Science.gov (United States)

    Persichetti, Paolo; Cagli, Barbara; Simone, Pierfranco; Cogliandro, Annalisa; Fortunato, Lucio; Altomare, Vittorio; Trodella, Lucio

    2009-04-01

    The most common surgical approach in case of local tumor recurrence after quadrantectomy and radiotherapy is salvage mastectomy. Breast reconstruction is the subsequent phase of the treatment and the plastic surgeon has to operate on previously irradiated and manipulated tissues. The medical literature highlights that breast reconstruction with tissue expanders is not a pursuable option, considering previous radiotherapy a contraindication. The purpose of this retrospective study is to evaluate the influence of previous radiotherapy on 2-stage breast reconstruction (tissue expander/implant). Only patients with analogous timing of radiation therapy and the same demolitive and reconstructive procedures were recruited. The results of this study prove that, after salvage mastectomy in previously irradiated patients, implant reconstruction is still possible. Further comparative studies are, of course, advisable to draw any conclusion on the possibility to perform implant reconstruction in previously irradiated patients.

  7. Comparison of piracetam measured with HPLC-DAD, HPLC-ESI-MS, DIP-APCI-MS, and a newly developed and optimized DIP-ESI-MS.

    Science.gov (United States)

    Lenzen, Claudia; Winterfeld, Gottfried A; Schmitz, Oliver J

    2016-06-01

    The direct inlet probe-electrospray ionization (DIP-ESI) presented here was based on the direct inlet probe-atmospheric pressure chemical ionization (DIP-APCI) developed by our group. It was coupled to an ion trap mass spectrometer (MS) for the detection of more polar compounds such as degradation products from pharmaceuticals. First, the position of the ESI tip, the gas and solvent flow rates, as well as the gas temperature were optimized with the help of the statistic program Minitab® 17 and a caffeine standard. The ability to perform quantitative analyses was also tested by using different concentrations of caffeine and camphor. Calibration curves with a quadratic calibration regression of R (2) = 0.9997 and 0.9998 for caffeine and camphor, respectively, were obtained. The limit of detection of 2.5 and 1.7 ng per injection for caffeine and camphor were determined, respectively. Furthermore, a solution of piracetam was used to compare established analytical methods for this drug and its impurities such as HPLC-diode array detector (DAD) and HPLC-ESI-MS with the DIP-APCI and the developed DIP-ESI. With HPLC-DAD and 10 μg piracetam on column, no impurity could be detected. With HPLC-ESI-MS, two impurities (A and B) were identified with only 4.6 μg piracetam on column, while with DIP-ESI, an amount of 1.6 μg piracetam was sufficient. In the case of the DIP-ESI measurements, all detected impurities could be identified by MS/MS studies. Graphical Abstract Scheme of the DIP-ESI principle.

  8. Detection of nonsterol isoprenoids by HPLC-MS/MS

    NARCIS (Netherlands)

    Henneman, Linda; van Cruchten, Arno G.; Denis, Simone W.; Amolins, Michael W.; Placzek, Andrew T.; Gibbs, Richard A.; Kulik, Willem; Waterham, Hans R.

    2008-01-01

    Isoprenoids constitute an important class of biomolecules that participate in many different cellular processes. Most available detection methods allow the identification of only one or two specific nonsterol isoprenoid intermediates following radioactive or fluorescent labeling. We here report a

  9. Screening and Analysis of the Potential Bioactive Components of Poria cocos (Schw. Wolf by HPLC and HPLC-MSn with the Aid of Chemometrics

    Directory of Open Access Journals (Sweden)

    Ling-Fang Wu

    2016-02-01

    Full Text Available The aim of the present study was to establish a new method based on Similarity Analysis (SA, Cluster Analysis (CA and Principal Component Analysis (PCA to determine the quality of different samples of Poria cocos (Schw. Wolf obtained from Yunnan, Hubei, Guizhou, Fujian, Henan, Guangxi, Anhui and Sichuan in China. For this purpose 15 samples from the different habitats were analyzed by HPLC-PAD and HPLC-MSn. Twenty-three compounds were detected by HPLC-MSn, of which twenty compounds were tentatively identified by comparing their retention times and mass spectrometry data with that of reference compounds and reviewing the literature. The characteristic fragmentations were summarized. 3-epi-Dehydrotumulosic acid (F13, 3-oxo-16α,25-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F4, 3-oxo-6,16α-dihydroxylanosta-7,9(11,24(31-trien-21-oic acid (F7 and dehydropachymic acid (F15 were deemed to be suitable marker compounds to distinguish between samples of different quality according to CA and PCA. This study provides helpful chemical information for further anti-tumor activity and active mechanism research on P. cocos. The results proved that fingerprint combined with a chemometric approach is a simple, rapid and effective method for the quality discrimination of P. cocos.

  10. Determination of boron in uranium and aluminium by high pressure liquid chromatography (HPLC)

    International Nuclear Information System (INIS)

    Rao, Radhika M.; Aggarwal, S.K.

    2003-01-01

    Experiments were conducted for the determination of boron in U 3 O 8 powder and aluminium metal using dynamically modified reversed phase high pressure liquid chromatography (RP-HPLC) and using precolumn chromogenic agent viz. curcumin for complexing boron. The complex was separated from the excess of reagent and determined by HPLC. The boron curcumin complex (rosocyanin) was formed after extraction of boron with 2-ethyl-1,3-hexane diol (EHD). Linear calibration curves for boron amounts in the range of 0.02 μg to 0.5 μg were developed and used for the determination of boron in aluminium and uranium samples. (author)

  11. Use of HPLC with flow-through radiometric detection for low level environmental analysis

    International Nuclear Information System (INIS)

    Mao, J.; Fackler, P.H.

    1992-01-01

    High Performance Liquid Chromatography with flow-through radiometric detection (HPLC-RAM) is increasingly becoming a standard analytical technique in pharmaceutical, agricultural and chemical industries for monitoring radiolabeled analytes. This paper focuses on the applications of this flow-through radiochromatographic technique for low level aquatic toxicology and environmental fate testing. Examples include parts per billion water, sediment/soil and fish tissue analyses using reverse phase as well as normal phase HPLC. The applications of both homogeneous (liquid) and heterogeneous (solid) flow cell scintillation counting are addressed. Compounds discussed are primarily pesticides and pharmaceuticals

  12. Pharmacokinetic study of arctigenin in rat plasma and organ tissue by RP-HPLC method.

    Science.gov (United States)

    He, Fan; Dou, De-Qiang; Hou, Qiang; Sun, Yu; Kang, Ting-Guo

    2013-01-01

    A high-performance liquid chromatography (HPLC) technique was developed for the determination of arctigenin in plasma and various organs of rats after the oral administration of 30, 50 and 70 mgkg(-1) of arctigenin to the Sprague-Dawley rats. Results showed that the validated HPLC method was simple, fast, reproducible and suitable to the determination of arctigenin in rat plasma and organ tissue and one-compartmental model with zero-order absorption process can well describe the changes of arctigenin concentration in the plasma. The concentration of compound was highest in the spleen, less in the liver and the least in the lung.

  13. [Study on HPLC-FPS of raw and processed fructus polygoni orientalis].

    Science.gov (United States)

    Zhai, Yanjun; Zhao, Min; Zhang, Hui; Chu, Zhengyun; Kang, Tingguo

    2010-03-01

    To establish the HPLC fingerprint method of Fructus Polygoni Orientalis before and after processed by choosing taxifolin as reference to compare the changes of chemical composition. HPLC method was emplyed with a gradient elution phase in a flow rate of 1 mL x min(-1) and the detection wavelength of 270 nm. Twenty marker peaks were marked out in the raw samples and 33 marker peaks in the processed product. Methodology met was consistent with the requirement, similarity was exceeded 0.9. This method is stationary, precise and feasible, which provide references of quality control for Fructus Polygoni Orientalis.

  14. A thin film degradation study of a fluorinated polyether liquid lubricant using an HPLC method

    Science.gov (United States)

    Morales, W.

    1986-01-01

    A High Pressure Liquid Chromatography (HPLC) separation method was developed to study and analyze a fluorinated polyether fluid which is promising liquid lubricant for future applications. This HPLC separation method was used in a preliminary study investigating the catalytic effect of various metal, metal alloy, and ceramic engineering materials on the degradation of this fluid in a dry air atmosphere at 345 C. Using a 440 C stainless steel as a reference catalytic material it was found that a titanium alloy and a chromium plated material degraded the fluorinated polyether fluid substantially more than the reference material.

  15. Principles of Developing Multi-Pesticide Methods Based on HPLC Determination

    Energy Technology Data Exchange (ETDEWEB)

    Dudar, E. [Plant Protection & Soil Conservation Service of Budapest, Budapest (Hungary)

    2009-07-15

    Principles for the development of multi-pesticide methods based on HPLC determination are outlined. Flow charts and block diagrams give guidance on how to proceed stepwise in the set-up of respective analytical methods. Detailed information is provided on what to take into consideration for setting up a pesticide formulation analysis method. HPLC variables like the types of column, solvents and their strength, pH value, eluent modifiers, column temperature, etc, and the influence on the separation and resolution of chromatographic peaks are discussed as well as the necessity and benefits of internal standardization. Examples of system suitability testing experiments are given for illustration. (author)

  16. 75 FR 54215 - Agency Request for Approval of a Previously Approved Information Collection(s): Uniform...

    Science.gov (United States)

    2010-09-03

    ... about our intention to request Office of Management and Budget (OMB) approval to renew a previously... because of management and oversight responsibilities of the agency imposed by OMB Circular 2 CFR 215 (A... Department has terminated Financial Status Report (SF-269 and SF-269A) and Federal Cash Transactions Report...

  17. HPLC-ED Analysis of Phenolic Compounds in Three Bosnian Crataegus Species

    Directory of Open Access Journals (Sweden)

    Dušan Čulum

    2018-04-01

    Full Text Available The aim of this work was the qualitative and quantitative determination of selected phenolic compounds in three Crataegus species grown in Bosnia. Crataegus plants are consumed for medicinal purposes and as foodstuff in the form of canned fruit, jam, jelly, tea, and wine. Two samples of plant material, dry leaves with flowers, and berries of three Crataegus species—Crataegus rhipidophylla Gand., Crataegus x subsphaericea Gand., and Crataegus x macrocarpa Hegetschw.—were analyzed. Twelve ethanolic extracts were isolated from the selected plant material using Soxhlet and ultrasound extraction, respectively. Soxhlet extraction proved to be more effective than ultrasound extraction. A simple and sensitive method, high-performance liquid chromatography with electrochemical detection, HPLC-ED, was used for the simultaneous determination of phenolic acids and flavonoids in Crataegus species. The content of gallic acid in the extracts ranged from 0.001 to 0.082 mg/g dry weight (DW, chlorogenic acid from 0.19 to 8.70 mg/g DW, and rutin from 0.03 to 13.49 mg/g DW. Two flavonoids, vitexin and hyperoside, commonly found in chemotaxonomic investigations of Crataegus species, were not detected in the examined extracts. In general, leaves with flowers samples are richer in gallic acid and rutin, whereas the berries samples are richer in chlorogenic acid. Distinct similarities were found in the relative distribution of gallic acid among the three species. Extracts of C. x macrocarpa had the highest content of all detected compounds, while significant differences were found in rutin content, depending on the plant organ. To the best of our knowledge, this is the first study reporting content of phenolic compounds in Crataegus rhipidophylla Gand., Crataegus x subsphaericea, and Crataegus x macrocarpa from Bosnia.

  18. Report to the CCT on COOMET comparison COOMET.T-K3.1 (previously COOMET.T-S1): Key regional comparison of the national standards of temperature in the range from the triple point of water to the freezing point of zinc

    Science.gov (United States)

    Pokhodun, A. I.

    2010-01-01

    In the framework of the CIPM MRA, a first COOMET comparison "Comparison of the ITS-90 realizations in the range from 0.01 °C to 429.7485 °C (from the triple point of water to the freezing point of zinc)", registered in the KCDB under the identifier "COOMET.T-K3", was carried out in 2005-2007. Four national metrology institutes took part in this comparison: VNIIM (Russian Federation), SMU (Slovakia), BelGIM (Republic of Belarus) and NSC IM (Ukraine), and two of them (VNIIM and SMU) ensured the linkage with key comparisons CCT-K3 and CCT-K4, in order to disseminate the metrological equivalence to the measurement standards of NSC IM and BelGIM. NSC IM, however, had to withdraw its results, and at the meeting of Technical Committee T-10 of COOMET it was decided to carry out a supplementary bilateral comparison between VNIIM and the NSC IM for realization of the ITS-90 in the same range of temperature. This was registered in the KCDB under the identifier COOMET.T-S1 and measurements were performed in 2008-2009. From the results presented in this report, it is possible to draw the conclusion that the COOMET supplementary comparison COOMET.T-S1 demonstrates the CMC uncertainties claimed by the NSC IM for the melting point of gallium 0.236 mK (k = 2), and the freezing points of indium 1.040 mK (k = 2), tin 0.858 mK (k = 2) and zinc 0.944 mK (k = 2). In September 2012 the Working Group on key Comparisons (WG 7) of the CCT upgraded this comparison to a COOMET key comparison of the 'CCT-K3' type. It is now identified as COOMET.T-K3.1. In April 2013 this report was superseded by item 03006 in the Technical Supplement of 2013. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCT, according to the provisions of the CIPM Mutual Recognition Arrangement (MRA).

  19. Personality disorders in previously detained adolescent females: a prospective study

    NARCIS (Netherlands)

    Krabbendam, A.; Colins, O.F.; Doreleijers, T.A.H.; van der Molen, E.; Beekman, A.T.F.; Vermeiren, R.R.J.M.

    2015-01-01

    This longitudinal study investigated the predictive value of trauma and mental health problems for the development of antisocial personality disorder (ASPD) and borderline personality disorder (BPD) in previously detained women. The participants were 229 detained adolescent females who were assessed

  20. Payload specialist Reinhard Furrer show evidence of previous blood sampling

    Science.gov (United States)

    1985-01-01

    Payload specialist Reinhard Furrer shows evidence of previous blood sampling while Wubbo J. Ockels, Dutch payload specialist (only partially visible), extends his right arm after a sample has been taken. Both men show bruises on their arms.

  1. Choice of contraception after previous operative delivery at a family ...

    African Journals Online (AJOL)

    Choice of contraception after previous operative delivery at a family planning clinic in Northern Nigeria. Amina Mohammed‑Durosinlorun, Joel Adze, Stephen Bature, Caleb Mohammed, Matthew Taingson, Amina Abubakar, Austin Ojabo, Lydia Airede ...

  2. Previous utilization of service does not improve timely booking in ...

    African Journals Online (AJOL)

    Previous utilization of service does not improve timely booking in antenatal care: Cross sectional study ... Journal Home > Vol 24, No 3 (2010) > ... Results: Past experience on antenatal care service utilization did not come out as a predictor for ...

  3. Arsenic speciation in biological environmental samples of aquatic ecosystems by using HPLC-ICP-MS; Speciation von Arsen in biologischen Umweltproben aus aquatischen Oekosystemen mittels HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Falk, K.

    1999-09-01

    The physicochemical forms of arsenic (arsenic species) which are present in the environment vary significantly with respect to toxicity, bioavailability, stability and transport behaviour. Therefore, it is necessary for an assessment of the toxic potential to humans and the environment to investigate not only the total arsenic concentrations but also to differentiate the single species. By that the knowledge about ecological correlations and pathways will be increased. The present thesis reports the results of a Ph.D. study on the development and optimisation of analytical methods for arsenic speciation and their application to biological samples from different aquatic ecosystems in Germany. The method development included separation of 12 naturally occurring arsenic species by high-performance liquid chromatography (HPLC) followed by an arsenic selective detection by inductively coupled plasma-mass spectrometry (ICP-MS). The arsenic species As (III), As (V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AB), arsenocholine (AC), trimethylarsine oxid (TMAO) and tetramethylarsonium (Tetra) were separated with ion-exchange chromatography, whereas reversed-phase chromatography was used for the separation of four arsenosugars. Because of the partly low arsenic concentration in biological samples a very good detection power was required. Therefore, an HPLC-ICP-MS system was tested with different nebulizers. Using the high efficiency nebulizer HHPN (Hydraulic High Pressure Nebulizer), detection limits in the low pg-range could be achieved. The developed analytical methods were applied to arsenic speciation in four marine matrices, which are representative of different trophic levels in the food chain. All samples originated from an ecosystem in the North Sea.

  4. A previous hamstring injury affects kicking mechanics in soccer players.

    Science.gov (United States)

    Navandar, Archit; Veiga, Santiago; Torres, Gonzalo; Chorro, David; Navarro, Enrique

    2018-01-10

    Although the kicking skill is influenced by limb dominance and sex, how a previous hamstring injury affects kicking has not been studied in detail. Thus, the objective of this study was to evaluate the effect of sex and limb dominance on kicking in limbs with and without a previous hamstring injury. 45 professional players (males: n=19, previously injured players=4, age=21.16 ± 2.00 years; females: n=19, previously injured players=10, age=22.15 ± 4.50 years) performed 5 kicks each with their preferred and non-preferred limb at a target 7m away, which were recorded with a three-dimensional motion capture system. Kinematic and kinetic variables were extracted for the backswing, leg cocking, leg acceleration and follow through phases. A shorter backswing (20.20 ± 3.49% vs 25.64 ± 4.57%), and differences in knee flexion angle (58 ± 10o vs 72 ± 14o) and hip flexion velocity (8 ± 0rad/s vs 10 ± 2rad/s) were observed in previously injured, non-preferred limb kicks for females. A lower peak hip linear velocity (3.50 ± 0.84m/s vs 4.10 ± 0.45m/s) was observed in previously injured, preferred limb kicks of females. These differences occurred in the backswing and leg-cocking phases where the hamstring muscles were the most active. A variation in the functioning of the hamstring muscles and that of the gluteus maximus and iliopsoas in the case of a previous injury could account for the differences observed in the kicking pattern. Therefore, the effects of a previous hamstring injury must be considered while designing rehabilitation programs to re-educate kicking movement.

  5. Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples

    Directory of Open Access Journals (Sweden)

    Amir Hooshang Mohammadpour

    2013-01-01

    Full Text Available Objective(s:The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. Materials and Methods:The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg cartridges or with direct precipitation using acetonitrile. Results:The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 – 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. Conclusion: The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study

  6. Quantitative fundus autofluorescence in mice: correlation with HPLC quantitation of RPE lipofuscin and measurement of retina outer nuclear layer thickness.

    Science.gov (United States)

    Sparrow, Janet R; Blonska, Anna; Flynn, Erin; Duncker, Tobias; Greenberg, Jonathan P; Secondi, Roberta; Ueda, Keiko; Delori, François C

    2013-04-17

    Our study was conducted to establish procedures and protocols for quantitative autofluorescence (qAF) measurements in mice, and to report changes in qAF, A2E bisretinoid concentration, and outer nuclear layer (ONL) thickness in mice of different genotypes and age. Fundus autofluorescence (AF) images (55° lens, 488 nm excitation) were acquired in albino Abca4(-/-), Abca4(+/-), and Abca4(+/+) mice (ages 2-12 months) with a confocal scanning laser ophthalmoscope (cSLO). Gray levels (GLs) in each image were calibrated to an internal fluorescence reference. The bisretinoid A2E was measured by quantitative high performance liquid chromatography (HPLC). Histometric analysis of ONL thicknesses was performed. The Bland-Altman coefficient of repeatability (95% confidence interval) was ±18% for between-session qAF measurements. Mean qAF values increased with age (2-12 months) in all groups of mice. qAF was approximately 2-fold higher in Abca4(-/-) mice than in Abca4(+/+) mice and approximately 20% higher in heterozygous mice. HPLC measurements of the lipofuscin fluorophore A2E also revealed age-associated increases, and the fold difference between Abca4(-/-) and wild-type mice was more pronounced (approximately 3-4-fold) than measurable by qAF. Moreover, A2E levels declined after 8 months of age, a change not observed with qAF. The decline in A2E levels in the Abca4(-/-) mice corresponded to reduced photoreceptor cell viability as reflected in ONL thinning beginning at 8 months of age. The qAF method enables measurement of in vivo lipofuscin and the detection of genotype and age-associated differences. The use of this approach has the potential to aid in understanding retinal disease processes and will facilitate preclinical studies.

  7. Simultaneous quantification by HPLC of the phenolic compounds for the crude drug of Prunus serotina subsp. capuli.

    Science.gov (United States)

    Rivero-Cruz, Blanca

    2014-08-01

    Prunus serotina Ehrenb. subsp. capuli (Cav.) McVaugh (Rosaceae), commonly known as "capulin", is a native North American tree, commercialized and used in folk medicine for the treatment of the hypertension, gastrointestinal illnesses, and cough. This work developed a suitable HPLC method for quantifying the major active constituents of the infusion of P. serotina, the most important preparation consumed by populations around the world. The analytical method was performed using a Fortis-RP column (150 mm × 4.6 mm; film thickness 5 µm). The mobile phase consisted of an isocratic acetate buffer solution (pH 2.7; A) and methanol (B) (65:35 v/v) at a flow rate of 1.0 mL min(-1). The proposed method was applied to the quantification of 1-3 in several samples of the leaves of P. serotina. The results indicated that amounts of 1-3 in the samples analyzed are uniform, and greater amounts of chlorogenic acid (2; 479.9 ± 33.6 µg g(-1), dry matter) along with hyperoside (1; 185.7 ± 55.3 µg g(-1), dry matter) were present. On the other hand, benzaldehyde (3; 118.2 ± 12.1 µg g(-1) dry matter) was found to be in lower concentration. A simple, sensitive, precise, and reproducible HPLC method for the simultaneous quantification of 1-3 in P. serotina was developed and validated. This is the first report on the quantification of 1-3 as active principles, and compound 1 was selected as a marker of P. serotina, which could be useful to guarantee the quality of the crude drug and herbal products.

  8. Isolation, characterization and HPLC quantification of compounds from Aquilegia fragrans Benth: Their in vitro antibacterial activities against bovine mastitis pathogens.

    Science.gov (United States)

    Mushtaq, Saleem; Aga, Mushtaq A; Qazi, Parvaiz H; Ali, Md Niamat; Shah, Aabid Manzoor; Lone, Sajad Ahmad; Shah, Aiyatullah; Hussain, Aehtesham; Rasool, Faheem; Dar, Hafizullah; Shah, Zeeshan Hamid; Lone, Shabir H

    2016-02-03

    The underground parts of Aquilegia fragrans are traditionally used for the treatment of wounds and various inflammatory diseases like bovine mastitis. However, there are no reports on the phytochemical characterization and antibacterial studies of A. fragrans. To isolate compounds from the methanol extract of the underground parts of A. fragrans and determine their antibacterial activity against the pathogens of bovine mastitis. The study was undertaken in order to scientifically validate the traditional use of A. fragrans. Five compounds were isolated from the methanol extract of the underground parts of A. fragrans using silica gel column chromatography. Structural elucidation of the isolated compounds was done using spectral data analysis and comparison with literature. High performance liquid chromatography (HPLC) was used for the qualitative and quantitative determination of isolated compounds in the crude methanol extract. The methanol extract and isolated compounds were evaluated for antibacterial activities against mastitis pathogens using broth micro-dilution technique. The five isolated compounds were identified as (1) 2, 4-dihydroxyphenylacetic acid methyl ester (2) β-sitosterol (3) Aquilegiolide (4) Glochidionolactone-A and (5) Magnoflorine. A quick and sensitive HPLC method was developed for the first time for qualitative and quantitative determination of four isolated marker compounds from A. fragrans. The crude methanol extract and compound 5 exhibited weak antibacterial activities that varied between the bacterial species (MIC=500-3000 µg/ml). The above results show that the crude methanol extract and isolated compounds from A. fragrans exhibit weak antibacterial activities. Further phytochemical and pharmacological studies are required for proper scientific validation of the folk use of this plant species in the treatment of various inflammatory diseases like bovine mastitis. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

  9. Chemometrics enhanced HPLC-DAD performance for rapid quantification of carbamazepine and phenobarbital in human serum samples.

    Science.gov (United States)

    Vosough, Maryam; Ghafghazi, Shiva; Sabetkasaei, Masoumeh

    2014-02-01

    This paper describes development and validation of a simple and efficient bioanalytical procedure for simultaneous determination of phenobarbital and carbamazepine in human serum samples using high performance liquid chromatography with photodiode-array detection (HPLC-DAD) regarding a fast elution methodology in less than 5 min. Briefly, this method consisted of a simple deproteinization step of serum samples followed by HPLC analysis on a Bonus-RP column using an isocratic mode of elution with acetonitrile/K2HPO4 (pH=7.5) buffer solution (45:55). Due to the presence of serum endogenous components as non-calibrated components in the sample, second-order calibration based on multivariate curve resolution-alternating least squares (MCR-ALS), has been applied on a set of absorbance matrices collected as a function of retention time and wavelengths. Acceptable resolution and quantification results were achieved in the presence of matrix interferences and the second-order advantage was fully exploited. The average recoveries for carbamazepine and phenobarbital were 89.7% and 86.1% and relative standard deviation values were lower than 9%. Additionally, computed elliptical joint confidence region (EJCR) confirmed the accuracy of the proposed method and indicated the absence of both constant and proportional errors in the predicted concentrations. The developed method enabled the determination of the analytes in different serum samples in the presence of overlapped profiles, while keeping experimental time and extraction steps at minimum. Finally, the serum concentration levels of carbamazepine in three time intervals were reported for morphine-dependents who had received carbamazepine for treating their neuropathic pain. © 2013 Elsevier B.V. All rights reserved.

  10. Application of ABTS radical cation for selective on-line detection of radical scavengers in HPLC eluates

    NARCIS (Netherlands)

    Koleva, [No Value; Niederlander, HAG; van Beek, TA

    2001-01-01

    The radical cation 2,2 ' -azinobis-(3 -ethylbenzothiazoline-6-sulfonate), (ABTS(.+)) was utilized in an on-line HPLC method for the detection of radical scavengers in complex matrixes. The HPLC-separated analytes react postcolumn with the preformed ABTS(.+), and the induced bleaching is detected as

  11. Competitive Nitration of Benzene-Fluorobenzene and Benzene-Toluene Mixtures: Orientation and Reactivity Studies Using HPLC

    Science.gov (United States)

    Blankespoor, Ronald L.; Hogendoorn, Stephanie; Pearson, Andrea

    2007-01-01

    The reactivity and orientation effects of a substituent are analyzed by using HPLC to determine the competitive nitration of the benzene-toluene and benzene-fluorobenzene mixtures. The results have shown that HPLC is an excellent instrumental method to use in analyzing these mixtures.

  12. The first use of a HPLC system at a Louisiana Sugarcane Factory: What it can do for you

    Science.gov (United States)

    Alma Plantation sugarcane factory established and operated the first High Performance Liquid Chromatography (HPLC) system in Louisiana in 2015. Although many HPLC systems exist, the factory opted for a ThermoFisherTM ion chromatography (anion exchange) system with integrated pulsed amperometric det...

  13. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Characterisation of oligosaccharides in vegetables by HPLC and MALDI-TOF MS

    Czech Academy of Sciences Publication Activity Database

    Štikarovská, M.; Chmelík, Josef

    96(S), - (2002), s. S189-S191 ISSN 0009-2770. [Meeting of Chemistry & Life /2./. Brno, 10.09.2002-11.09.2002] Institutional research plan: CEZ:AV0Z4031919 Keywords : oligosaccharides * HPLC * MALDI-TOF-MS Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.336, year: 2002

  15. Quantitative HPLC analysis of some marker compounds of hydroalcoholic extracts of Piper aduncum L

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Laura C.P.; Nunomura, Sergio M. [Instituto Nacional de Pesquisas da Amazonia (INPA), Manaus, AM (Brazil). Coordenacao de Pesquisas em Produtos Naturais]. E-mail: smnunomu@inpa.gov.br; Mause, Robert [Siema Eco Essencias da Amazonia Ltda., Manaus, AM (Brazil)

    2005-11-15

    High performance liquid chromatography is one of the major analytical techniques used in the quality control of phytotherapics. This work describes a HPLC method used to determine the major components present in different hydroalcoholic extracts of aerial parts of Piper aduncum. (author)

  16. A Decomposition Model for HPLC-DAD Data Set and Its Solution by Particle Swarm Optimization

    Directory of Open Access Journals (Sweden)

    Lizhi Cui

    2014-01-01

    Full Text Available This paper proposes a separation method, based on the model of Generalized Reference Curve Measurement and the algorithm of Particle Swarm Optimization (GRCM-PSO, for the High Performance Liquid Chromatography with Diode Array Detection (HPLC-DAD data set. Firstly, initial parameters are generated to construct reference curves for the chromatogram peaks of the compounds based on its physical principle. Then, a General Reference Curve Measurement (GRCM model is designed to transform these parameters to scalar values, which indicate the fitness for all parameters. Thirdly, rough solutions are found by searching individual target for every parameter, and reinitialization only around these rough solutions is executed. Then, the Particle Swarm Optimization (PSO algorithm is adopted to obtain the optimal parameters by minimizing the fitness of these new parameters given by the GRCM model. Finally, spectra for the compounds are estimated based on the optimal parameters and the HPLC-DAD data set. Through simulations and experiments, following conclusions are drawn: (1 the GRCM-PSO method can separate the chromatogram peaks and spectra from the HPLC-DAD data set without knowing the number of the compounds in advance even when severe overlap and white noise exist; (2 the GRCM-PSO method is able to handle the real HPLC-DAD data set.

  17. Two Validated HPLC Methods for the Quantification of Alizarin and other Anthraquinones in Rubia tinctorum Cultivars

    NARCIS (Netherlands)

    Derksen, G.C.H.; Lelyveld, G.P.; Beek, van T.A.; Capelle, A.; Groot, de Æ.

    2004-01-01

    Direct and indirect HPLC-UV methods for the quantitative determination of anthraquinones in dried madder root have been developed, validated and compared. In the direct method, madder root was extracted twice with refluxing ethanol-water. This method allowed the determination of the two major native

  18. A simple method for HPLC retention time prediction: linear calibration using two reference substances.

    Science.gov (United States)

    Sun, Lei; Jin, Hong-Yu; Tian, Run-Tao; Wang, Ming-Juan; Liu, Li-Na; Ye, Liu-Ping; Zuo, Tian-Tian; Ma, Shuang-Cheng

    2017-01-01

    Analysis of related substances in pharmaceutical chemicals and multi-components in traditional Chinese medicines needs bulk of reference substances to identify the chromatographic peaks accurately. But the reference substances are costly. Thus, the relative retention (RR) method has been widely adopted in pharmacopoeias and literatures for characterizing HPLC behaviors of those reference substances unavailable. The problem is it is difficult to reproduce the RR on different columns due to the error between measured retention time (t R ) and predicted t R in some cases. Therefore, it is useful to develop an alternative and simple method for prediction of t R accurately. In the present study, based on the thermodynamic theory of HPLC, a method named linear calibration using two reference substances (LCTRS) was proposed. The method includes three steps, procedure of two points prediction, procedure of validation by multiple points regression and sequential matching. The t R of compounds on a HPLC column can be calculated by standard retention time and linear relationship. The method was validated in two medicines on 30 columns. It was demonstrated that, LCTRS method is simple, but more accurate and more robust on different HPLC columns than RR method. Hence quality standards using LCTRS method are easy to reproduce in different laboratories with lower cost of reference substances.

  19. Apparent loss of urinary albumin during long-term frozen storage : HPLC vs immunonephelometry

    NARCIS (Netherlands)

    Brinkman, Jacoline W.; De Zeeuw, Dick; Lambers Heerspink, Hiddo J.; Gansevoort, Ronald T.; Kema, Ido P.; de Jong, Paul E.; Bakker, Stephan J. L.

    Background: Urinary albumin detection by immuno-nephelometry is decreased by -30% in samples that have been frozen at -20 degrees C. An HPLC method for assessment of urinary albumin that detects immunoreactive and immunochemically nonreactive albumin has been introduced as an alternative to

  20. Quantitative HPLC analysis of some marker compounds of hydroalcoholic extracts of Piper aduncum L

    International Nuclear Information System (INIS)

    Oliveira, Laura C.P.; Nunomura, Sergio M.

    2005-01-01

    High performance liquid chromatography is one of the major analytical techniques used in the quality control of phytotherapics. This work describes a HPLC method used to determine the major components present in different hydroalcoholic extracts of aerial parts of Piper aduncum. (author)

  1. A NEW HPLC METHOD FOR SEPARATION OF PHYTOPLANKTON PIGMENTS IN NATURAL SAMPLES

    Science.gov (United States)

    A new high-performance liquid chromatographic (HPLC) method was developed to analyze, in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a reverse-phase amide C16 (RP-amide C16) column and an elution gradient o...

  2. An optimized method for automated analysis of algal pigments by HPLC

    NARCIS (Netherlands)

    van Leeuwe, M. A.; Villerius, L. A.; Roggeveld, J.; Visser, R. J. W.; Stefels, J.

    2006-01-01

    A recent development in algal pigment analysis by high-performance liquid chromatography (HPLC) is the application of automation. An optimization of a complete sampling and analysis protocol applied specifically in automation has not yet been performed. In this paper we show that automation can only

  3. Melanin determination by high performance liquid chromatography (HPLC) for K. marxianus

    Science.gov (United States)

    Ultraviolet light (UV) mutated K. marxianus was found to turn dark brown during a growth assay. This brown color was hypothesized to be melanin overproduction influenced by the UV exposure. Cell cultures were oxidized and HPLC analyzed to determine melanin concentrations. The resulting melanin con...

  4. Simultaneous analysis of 17 diuretics in dietary supplements by HPLC and LC-MS/MS.

    Science.gov (United States)

    Woo, H; Kim, J W; Han, K M; Lee, J H; Hwang, I S; Lee, J H; Kim, J; Kweon, S J; Cho, S; Chae, K R; Han, S Y; Kim, J

    2013-01-01

    In order to test health foods for illegally added diuretics for weight loss, we developed simple, rapid, selective, and sensitive methods using HPLC and LC-MS/MS for the simultaneous analysis of 17 diuretics in dietary supplements. HPLC conditions were set with a Capcell-pak C18, using a mobile phase consisting of gradient conditions, UV detection at 254 nm and validated for linearity (r(2)> 0.999), precision (CV ≤ 3%), recoveries (90.4-102.8%) and reproducibility. Identification and quantification of 17 diuretics were accomplished by ion-spray LC-MS/MS using multiple reaction monitoring (MRM). The chromatographic separation was carried out under the reversed-phase mechanism on an HSS-T3 column. The LC-MS/MS method was validated for linearity (r(2)> 0.99) and precision (CV Diuretics were not detected in all samples. Extraction recovery was also investigated and the extraction recoveries in different formulations were from 88% to 110% and from 81% to 116% using HPLC and LC-MS/MS, respectively. There was no significant difference in recoveries in the type of dietary supplements. Based on this result, the developed methods to monitor illegal drug adulterations in dietary supplements using HPLC and LC-MS/MS are simple, fast and reliable. Therefore, it is applicable to routine drug-adulteration screening.

  5. 2D-HPLC and MALDI-TOF/TOF analysis of barley proteins glycated during brewing

    Czech Academy of Sciences Publication Activity Database

    Petry-Podgorska, Inga; Žídková, Jitka; Flodrová, Dana; Bobálová, Janette

    2010-01-01

    Roč. 878, č. 30 (2010), s. 3143-3148 ISSN 1570-0232 R&D Projects: GA MŠk 1M0570 Institutional research plan: CEZ:AV0Z40310501 Keywords : 2D-HPLC * MALDI-TOF/TOF mass spectrometry * barley Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.971, year: 2010

  6. Determination of epirubicin and its metabolite epirubicinol in saliva and plasma by HPLC

    NARCIS (Netherlands)

    Dodde, WIW; Maring, JG; Hendriks, G; Wachters, FM; Groen, HJM; de Vries, EGE; Uges, DRA

    We present a high-performance liquid chromatography (HPLC) method suitable for the analysis of epirubicin and its metabolite epirubicinol in saliva and plasma. Preparation of saliva and plasma samples was performed by extraction of analytes with a chloroform: 2-propanol mixture (6:1, vol/vol) and

  7. Determination of organic acids evolution during apple cider fermentation using an improved HPLC analysis method

    NARCIS (Netherlands)

    Zhang, H.; Zhou, F.; Ji, B.; Nout, M.J.R.; Fang, Q.; Zhang, Z.

    2008-01-01

    An efficient method for analyzing ten organic acids in food, namely citric, pyruvic, malic, lactic, succinic, formic, acetic, adipic, propionic and butyric acids, using HPLC was developed. Boric acid was added into the mobile phase to separate lactic and succinic acids, and a post-column buffer

  8. Screening natural antioxidants in peanut shell using DPPH-HPLC-DAD-TOF/MS methods.

    Science.gov (United States)

    Qiu, Jiying; Chen, Leilei; Zhu, Qingjun; Wang, Daijie; Wang, Wenliang; Sun, Xin; Liu, Xiaoyong; Du, Fangling

    2012-12-15

    Peanut shell, a byproduct in oil production, is rich in natural antioxidants. Here, a rapid and efficient method using DPPH-HPLC-DAD-TOF/MS was used for the first time to screen antioxidants in peanut shell. The method is based on the hypothesis that upon reaction with 1, 1-diphenyl-2-picrylhydrazyl (DPPH), the peak areas of compounds with potential antioxidant activities in the HPLC chromatogram will be significantly reduced or disappeared, and the identity confirmation could be achieved by HPLC-DAD-TOF/MS technique. With this method, three compounds possessing potential antioxidant activities were found abundantly in the methanolic extract of peanut shell. They were identified as 5,7-dihydroxychromone, eriodictyol, and luteolin. The contents of these compounds were 0.59, 0.92, and 2.36 mg/g, respectively, and luteolin possessed the strongest radical scavenging capacity. DPPH-HPLC-DAD-TOF/MS assay facilitated rapid identification and determination of natural antioxidants in peanut shell, which may be helpful for value-added utilization of peanut processing byproducts. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Simultaneous HPLC quantitative analysis of mangostin derivatives in Tetragonula pagdeni propolis extracts

    Directory of Open Access Journals (Sweden)

    Sumet Kongkiatpaiboon

    2016-04-01

    Full Text Available Propolis has been used as indigenous medicine for curing numerous maladies. The one that is of ethnopharmacological use is stingless bee propolis from Tetragonula pagdeni. A simultaneous high-performance liquid chromatography (HPLC investigation was developed and validated to determine the contents of bioactive compounds: 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin. HPLC analysis was effectively performed using a Hypersil BDS C18 column, with the gradient elution of methanol–0.2% formic acid and a flow rate of 1 ml/min, at 25 °C and detected at 245 nm. Parameters for the validation included accuracy, precision, linearity, and limits of quantitation and detection. The developed HPLC technique was precise, with lower than 2% relative standard deviation. The recovery values of 3-isomangostin, gamma-mangostin, beta-mangostin, and alpha-mangostin in the extracts were 99.98%, 99.97%, 98.98% and 99.19%, respectively. The average contents of these mixtures in the propolis extracts collected from different seasons were 0.127%, 1.008%, 0.323% and 2.703% (w/w, respectively. The developed HPLC technique was suitable and practical for the simultaneous analysis of these mangostin derivatives in T. pagdeni propolis and would be a valuable guidance for the standardization of its pharmaceutical products.

  10. HPLC-photodiode array detection analysis of curcuminoids in Curcuma species indigenous to Indonesia

    NARCIS (Netherlands)

    Bos, Rein; Windono, Tri; Woerdenbag, Herman J.; Boersma, Ykelien L.; Koulman, Albert; Kayser, Oliver

    An optimized HPLC method with photodiode array detection was developed and applied to analyse the curcuminoids curcumin, demethoxycurcumin, and bis-demethoxycurcumin in rhizomes of Curcuma mangga Val &. v. Zijp, C. heyneana Val. & v. Zijp, C. aeruginosa Roxb. and C. soloensis Val. (Zingiberaceae),

  11. Determination of acetylsalicylic acid and salicylic acid in foods, using HPLC with fluorescence detection.

    NARCIS (Netherlands)

    Venema, D.P.; Hollman, P.C.H.; Janssen, P.L.T.M.K.; Katan, M.B.

    1996-01-01

    We developed a specific and sensitive HPLC method with fluorescence detection for the determination of free acetylsalicylic acid, free salicylic acid, and free salicylic acid plus salicylic acid after alkaline hydrolysis (free-plus-bound) in foods. Acetylsalicylic acid was detected after postcolumn

  12. Application of HPLC capacity coefficients to characterize the sorption of polycyclic aromatic compounds to humic acid

    DEFF Research Database (Denmark)

    Nielsen, T.; Helweg, C.; Siigur, K.

    1997-01-01

    The sorption coefficients to humic acid of 46 PAC having a wide range in polarity were compared with the capacity coefficients of the PAC to a non-polar HPLC column material (ODS) and a polar one (Diol). It is shown that polar interactions contribute to the sorption of polar PAC in addition...

  13. Determination of Trace Level Triclosan in Water by Online Preconcentration and HPLC-UV Diode Array

    Science.gov (United States)

    An online high performance liquid chromatography (HPLC) method for the detection and quantification of trace levels of triclosan in water is discussed. Triclosan, an anti-bacterial agent, and related compounds have been shown to reach municipal waste waters through the disposal ...

  14. Time-resolved SAXS measurements facilitated by online HPLC buffer exchange

    DEFF Research Database (Denmark)

    Jensen, Malene Hillerup; Toft, Katrine Nørgaard; David, Gabriel

    2010-01-01

    continuous or stopped flow. In this paper a method for obtaining TR-SAXS data from systems where the reaction is triggered by removal of a species is presented. This method is based on fast buffer exchange over a short desalting column facilitated by an online HPLC (high-performance liquid chromatography...

  15. SEPARATION OF OCTYLPHENOL POLYETHER ALCOHOLS SURFACTANTS BY CAPILLARY COLUMN SFC AND HPLC

    Science.gov (United States)

    Separation of nonionic octylphenol polyether alcohols (OPA) by supercritical fluid chromatography (SFC) and HPLC is described. Using a density programming and a 50-μm i.d. capillary column, a total of 18 group oligomers was separated. The effects of the operating parameters, such...

  16. An introduction of HPLC to check contamination in the adsorption of uranium from sea water

    International Nuclear Information System (INIS)

    Takai, Nobuharu; Senoo, Manabu; Sugasaka, Kazuhiko; Katoh, Shunsaku; Ouchi, Hideyoshi; Itagaki, Takaharu.

    1984-01-01

    Seawater contains many inorganic ions and many organic substances, and they are adsorbed by adsorbents as well as uranium, and some of which are released into solution when desorbed. An examination was carried out on the substances contained in desorption solution using HPLC to confirm the desorption behavior of contaminants. The instruments used for the test were Hitachi HPLC Model 638 and the prototype spectrophotometer with 32 wave lengths, and the signals from the spectrophotometer are transmitted to a microcomputer through I/O. The test was carried out at National Industrial Institute of Shikoku using the desorption solution obtained from the composite adsorbent of carbon titanium and amidoxime resin by the treatment with acid and alkali. As preliminary test, desorption behavior was detected with the HPLC on the samples of various desorption solutions with a detector of fixed wave length at various wave lengths. Another test was carried out using the prototype with 32 wave lengths to check the function of the system. Desorption solution was tested with the HPLC with the detector of multi-wave lengths. From the experimental results, it was found that the contaminants contained in acid desorption solution were largely different from those contained in sodium carbonate desorption solution. (Yoshitake, I.)

  17. Extraction and Purification of Glucoraphanin by Preparative High-Performance Liquid Chromatography (HPLC)

    Science.gov (United States)

    Lee, Iris; Boyce, Mary C.

    2011-01-01

    A student activity that focuses on the isolation of glucoraphanin from broccoli using preparative high-performance liquid chromatography (HPLC) is presented here. Glucoraphanin is a glucosinolate, whose byproducts are known to possess anticancer properties. It is present naturally at high levels in broccoli and other "Brassica" vegetables. This…

  18. Analysis of several irdoid and indole precursors of terpenoid indole alkaloids with a single HPLC run

    DEFF Research Database (Denmark)

    Dagnino, Denise; Schripsema, Jan; Verpoorte, Robert

    1996-01-01

    An isocratic HPLC system is described which allows the separation of the iridoid and indole precursors of terpenoid indole alkaloids, which are present in a single crude extract. The system consists of a column of LiChrospher 60 RP select B 5 my, 250x4 mm (Merck) with an eluent of 1 % formic acid...

  19. A first step towards miniaturized HPLC systems in analytical routine laboratories

    NARCIS (Netherlands)

    Straten, van M.A.; Vermeer, E.A.; Claessens, H.A.

    1996-01-01

    This article shows that the first step towards the miniaturization of HPLC systems can be made without any, or only slight, modification to conventional equipment. Minor (less expensive) equipment modifications, particularly the use of micro-detector cells, allow the routine use of 3.2- and 2.1-mm

  20. Using HPLC-Mass Spectrometry to Teach Proteomics Concepts with Problem-Based Techniques

    Science.gov (United States)

    Short, Michael; Short, Anne; Vankempen, Rachel; Seymour, Michael; Burnatowska-Hledin, Maria

    2010-01-01

    Practical instruction of proteomics concepts was provided using high-performance liquid chromatography coupled with a mass selective detection system (HPLC-MS) for the analysis of simulated protein digests. The samples were prepared from selected dipeptides in order to facilitate the mass spectral identification. As part of the prelaboratory…

  1. Discrimination of Polish unifloral honeys using overall PTR-MS and HPLC fingerprints combined with chemometrics

    NARCIS (Netherlands)

    Kus, P.M.; Ruth, van S.M.

    2015-01-01

    A total of 62 honey samples of six floral origins (rapeseed, lime, heather, cornflower, buckwheat and black locust) were analysed by means of proton transfer reaction mass spectrometry (PTR-MS) and HPLC-DAD. The data were evaluated by principal component analysis and k-nearest neighbours

  2. Fluorescence detection of flavonols in HPLC by postcolumn chelation with aluminum

    NARCIS (Netherlands)

    Hollman, Peter C H; Van Trijp, J. M P; Buysman, Michel N C P

    1996-01-01

    Flavonols are dietary antioxidants which may prevent coronary heart disease. To be able to study absorption of flavonols in humans, we developed a postcolumn derivatization with aluminum for HPLC with fluorescence detection. Variables governing postcolumn chelation, such as water content, buffer,

  3. Comparison of calorimetric and HPLC methods in measuring nitrate content of meat products: An economic evaluation

    Directory of Open Access Journals (Sweden)

    M moradi

    2014-02-01

    Full Text Available Nitrate is a flavors compound, color stabilizer and growth inhibitor of anaerobic microorganisms in meat products. High concentration of nitrate in food can cause methaemoglobinaemia and is recognized as carcinogenic. Therefore, accurate determination of nitrate is crucial to ensure consumers’ health. Regularly, nitrate is estimated by colorimetric and HPLC methods. In measurement of nitrate, the efficiency, accuracy, speed and amount of material are important from economical point of view. In this study, the cost of initial investment, staff, consumable material and equipments used by the two methods were calculated and finally Net Present Value (NPV was estimated for each of them. The rate of interest was considered from 4 until 30%. According to the results the amount of initial investment, annual cost of staff and consumable materials for colorimetric method were determined as 274000000, 379080000 and 214289130 Rials, respectively. These costs for HPLC method were 342000000, 252720000 and 7633080 Rials, respectively. NPV in minimum and maximum rates of interest (4 and 30% for colorimetric method were 8368344000 and 2242330000 Rials and for HPLC method were estimated at 4035848000 and 1207544000 Rials. As a consequence, HPLC is more economical and could be recommended for the routine measurement of nitrate in of food safety laboratories.

  4. Determination of the sugar content in fruit flavoured drinks by HPLC ...

    African Journals Online (AJOL)

    The remaining 3 fruit flavoured drinks indicated the presence of glucose and sucrose only. The sugar content of some of the drinks calls for caution in children's diet especially with the rise in obesity and dental erosion in tooth enamel associated with sugar sweetened beverages or drinks. Keywords: HPLC; Fruit drinks, ...

  5. High-resolution α-glucosidase inhibition profiling combined with HPLC-HRMS-SPE-NMR for identification of anti-diabetic compounds in Eremanthus crotonoides (Asteraceae)

    DEFF Research Database (Denmark)

    Lana e Silva, Eder; Felipe Revoredo Lobo, Jonathas; Vinther, Joachim Møllesøe

    2016-01-01

    with an inhibitory concentration (IC50) of 34.5 μg/mL towards α-glucosidase was investigated by high-resolution α-glucosidase inhibition profiling combined with HPLC-HRMS-SPE-NMR. This led to identification of six α-glucosidase inhibitors, namely quercetin (16), trans-tiliroside (17), luteolin (19), quercetin-3.......93 and 5.20 μM, respectively. This is the first report of the α-glucosidase inhibitory activity of compounds 20, 26, and 29, and the findings support the important role of Eremanthus species as novel sources of new drugs and/or herbal remedies for treatment of type 2 diabetes....

  6. Efficient preparation of incensole and incensole acetate, and quantification of these bioactive diterpenes in Boswellia papyrifera by a RP-DAD-HPLC method.

    Science.gov (United States)

    Paul, Michael; Jauch, Johann

    2012-03-01

    Incensole and incensole acetate, found in incense, are encouraging potent bioactive diterpenic cembrenoids, inhibiting Nuclear Factor-kappaB activation. Furthermore, incensole acetate elicits psycho-activity in mice by activating the TRPV3 channels in the brain. Starting from crude extracts of the incense species Boswellia papyrifera Hochst., a convenient procedure for the efficient large-scale synthesis of incensole and its acetate is presented. Additionally, a reversed-phase, diode-array-detection, high-performance liquid chromatography (RP-DAD-HPLC) method for the quantification of incensole and incensole acetate is reported, indicating that these two compounds are typical biomarkers for B. papyrifera.

  7. Erlotinib-induced rash spares previously irradiated skin

    International Nuclear Information System (INIS)

    Lips, Irene M.; Vonk, Ernest J.A.; Koster, Mariska E.Y.; Houwing, Ronald H.

    2011-01-01

    Erlotinib is an epidermal growth factor receptor inhibitor prescribed to patients with locally advanced or metastasized non-small cell lung carcinoma after failure of at least one earlier chemotherapy treatment. Approximately 75% of the patients treated with erlotinib develop acneiform skin rashes. A patient treated with erlotinib 3 months after finishing concomitant treatment with chemotherapy and radiotherapy for non-small cell lung cancer is presented. Unexpectedly, the part of the skin that had been included in his previously radiotherapy field was completely spared from the erlotinib-induced acneiform skin rash. The exact mechanism of erlotinib-induced rash sparing in previously irradiated skin is unclear. The underlying mechanism of this phenomenon needs to be explored further, because the number of patients being treated with a combination of both therapeutic modalities is increasing. The therapeutic effect of erlotinib in the area of the previously irradiated lesion should be assessed. (orig.)

  8. Reasoning with Previous Decisions: Beyond the Doctrine of Precedent

    DEFF Research Database (Denmark)

    Komárek, Jan

    2013-01-01

    in different jurisdictions use previous judicial decisions in their argument, we need to move beyond the concept of precedent to a wider notion, which would embrace practices and theories in legal systems outside the Common law tradition. This article presents the concept of ‘reasoning with previous decisions...... law method’, but they are no less rational and intellectually sophisticated. The reason for the rather conceited attitude of some comparatists is in the dominance of the common law paradigm of precedent and the accompanying ‘case law method’. If we want to understand how courts and lawyers......’ as such an alternative and develops its basic models. The article first points out several shortcomings inherent in limiting the inquiry into reasoning with previous decisions by the common law paradigm (1). On the basis of numerous examples provided in section (1), I will present two basic models of reasoning...

  9. [Prevalence of previously diagnosed diabetes mellitus in Mexico.

    Science.gov (United States)

    Rojas-Martínez, Rosalba; Basto-Abreu, Ana; Aguilar-Salinas, Carlos A; Zárate-Rojas, Emiliano; Villalpando, Salvador; Barrientos-Gutiérrez, Tonatiuh

    2018-01-01

    To compare the prevalence of previously diagnosed diabetes in 2016 with previous national surveys and to describe treatment and its complications. Mexico's national surveys Ensa 2000, Ensanut 2006, 2012 and 2016 were used. For 2016, logistic regression models and measures of central tendency and dispersion were obtained. The prevalence of previously diagnosed diabetes in 2016 was 9.4%. The increase of 2.2% relative to 2012 was not significant and only observed in patients older than 60 years. While preventive measures have increased, the access to medical treatment and lifestyle has not changed. The treatment has been modified, with an increase in insulin and decrease in hypoglycaemic agents. Population aging, lack of screening actions and the increase in diabetes complications will lead to an increase on the burden of disease. Policy measures targeting primary and secondary prevention of diabetes are crucial.

  10. Activity behavior of a HPLC column including α-chymotrypsin immobilized monosized-porous particles

    International Nuclear Information System (INIS)

    Bilici, Z.; Camli, S.T.; Unsal, E.; Tuncel, A.

    2004-01-01

    In this study, a polymer-based, α-chymotrypsin (CT) immobilized HPLC column was prepared as a potential material for affinity-HPLC and chiral separation applications. Monosized-macroporous particles were synthesized as the support material by a relatively new polymerization protocol, the so-called, 'modified seeded polymerization'. The particles were obtained in the form of styrene-glycidyl methacrylate- divinylbenzene terpolymer approximately 11 μm in size. The particles were treated with aqueous ammonia to have primary amine groups on the porous surface. The amine functionalized particles were reacted by glutaraldehyde and the enzyme, CT, was covalently attached. CT carrying monosized-porous particles were slurry packed into the HPLC column 50 mmx4.6 mm in size. Since the activity behavior of immobilized CT played an important role in the enantiomeric separations performed by similar columns, the enzymatic activity behavior of the column produced by our protocol was determined. For this purpose, HPLC column was used as a packed bed reactor and the enzymatic reaction was continuously followed by measuring the absorbance of the output flow by the UV-detector of HPLC. S-shaped absorbance-time curves were obtained by monitoring the reactor output both in dynamic and steady-state periods. The columns with relatively lower immobilized enzyme content were more sensitive to the changes in the operating conditions and responded with more appreciable substrate conversion changes. The maximum reaction rate of the immobilized enzyme was estimated as approximately 25% of the free one by the mathematical model describing the activity behavior of the column. No significant loss was observed in the activity of the immobilized enzyme during the course of the experiments

  11. Determination of Bortezomib in API Samples Using HPLC: Assessment of Enantiomeric and Diastereomeric Impurities.

    Science.gov (United States)

    Kamalzadeh, Zahra; Babanezhad, Esmaeil; Ghaffari, Solmaz; Mohseni Ezhiyeh, Alireza; Mohammadnejad, Mahdieh; Naghibfar, Mehdi; Bararjanian, Morteza; Attar, Hossein

    2017-08-01

    A new, normal phase high performance liquid chromatography (NP-HPLC) method was developed for separation of Bortezomib (BZB) enantiomers and quantitative determination of (1S,2R)-enantiomer of BZB in active pharmaceutical ingredient (API) samples. The developed method was validated based on International Conference on Harmonisation (ICH) guidelines and it was proved to be accurate, precise and robust. The obtained resolution (RS) between the enantiomers was more than 2. The calibration curve for (1S,2R)-enantiomer was found to be linear in the concentration range of 0.24-5.36 mg/L with regression coefficient (R2) of 0.9998. Additionally, the limit of detection (LOD) and limit of quantification (LOQ) were 0.052 and 0.16 mg/L, respectively. Also, in this study, a precise, sensitive and robust gradient reversed-phase HPLC (RP-HPLC) method was developed and validated for determination of BZB in API samples. The detector response was linear over the concentration range of 0.26-1110.5 mg/L. The values of R2, LOD and LOQ were 0.9999, 0.084 and 0.25 mg/L, respectively. For both NP-HPLC and RP-HPLC methods, all of the RSD (%) values obtained in the precision study were 2,000 and RS > 2.0. The performance of two common integration methods of valley to valley and drop perpendicular for drawing the baseline between two adjacent peaks were investigated for the determination of diastereomeric impurity (Imp-D) in the BZB-API samples. The results showed that the valley to valley method outperform the drop perpendicular method for calculation of Imp-D peak areas. Therefore, valley to valley method was chosen for peak integration. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Cardiovascular magnetic resonance in adults with previous cardiovascular surgery.

    Science.gov (United States)

    von Knobelsdorff-Brenkenhoff, Florian; Trauzeddel, Ralf Felix; Schulz-Menger, Jeanette

    2014-03-01

    Cardiovascular magnetic resonance (CMR) is a versatile non-invasive imaging modality that serves a broad spectrum of indications in clinical cardiology and has proven evidence. Most of the numerous applications are appropriate in patients with previous cardiovascular surgery in the same manner as in non-surgical subjects. However, some specifics have to be considered. This review article is intended to provide information about the application of CMR in adults with previous cardiovascular surgery. In particular, the two main scenarios, i.e. following coronary artery bypass surgery and following heart valve surgery, are highlighted. Furthermore, several pictorial descriptions of other potential indications for CMR after cardiovascular surgery are given.

  13. Outcome Of Pregnancy Following A Previous Lower Segment ...

    African Journals Online (AJOL)

    Background: A previous ceasarean section is an important variable that influences patient management in subsequent pregnancies. A trial of vaginal delivery in such patients is a feasible alternative to a secondary section, thus aiding to reduce the ceasarean section rate and its associated co-morbidities. Objective: To ...

  14. 24 CFR 1710.552 - Previously accepted state filings.

    Science.gov (United States)

    2010-04-01

    ... of Substantially Equivalent State Law § 1710.552 Previously accepted state filings. (a) Materials... and contracts or agreements contain notice of purchaser's revocation rights. In addition see § 1715.15..., unless the developer is obligated to do so in the contract. (b) If any such filing becomes inactive or...

  15. The job satisfaction of principals of previously disadvantaged schools

    African Journals Online (AJOL)

    The aim of this study was to identify influences on the job satisfaction of previously disadvantaged ..... I am still riding the cloud … I hope it lasts. .... as a way of creating a climate and culture in schools where individuals are willing to explore.

  16. Research Note Effects of previous cultivation on regeneration of ...

    African Journals Online (AJOL)

    We investigated the effects of previous cultivation on regeneration potential under miombo woodlands in a resettlement area, a spatial product of Zimbabwe's land reforms. We predicted that cultivation would affect population structure, regeneration, recruitment and potential grazing capacity of rangelands. Plant attributes ...

  17. Cryptococcal meningitis in a previously healthy child | Chimowa ...

    African Journals Online (AJOL)

    An 8-year-old previously healthy female presented with a 3 weeks history of headache, neck stiffness, deafness, fever and vomiting and was diagnosed with cryptococcal meningitis. She had documented hearing loss and was referred to tertiary-level care after treatment with fluconazole did not improve her neurological ...

  18. Investigation of previously derived Hyades, Coma, and M67 reddenings

    International Nuclear Information System (INIS)

    Taylor, B.J.

    1980-01-01

    New Hyades polarimetry and field star photometry have been obtained to check the Hyades reddening, which was found to be nonzero in a previous paper. The new Hyades polarimetry implies essentially zero reddening; this is also true of polarimetry published by Behr (which was incorrectly interpreted in the previous paper). Four photometric techniques which are presumed to be insensitive to blanketing are used to compare the Hyades to nearby field stars; these four techniques also yield essentially zero reddening. When all of these results are combined with others which the author has previously published and a simultaneous solution for the Hyades, Coma, and M67 reddenings is made, the results are E (B-V) =3 +- 2 (sigma) mmag, -1 +- 3 (sigma) mmag, and 46 +- 6 (sigma) mmag, respectively. No support for a nonzero Hyades reddening is offered by the new results. When the newly obtained reddenings for the Hyades, Coma, and M67 are compared with results from techniques given by Crawford and by users of the David Dunlap Observatory photometric system, no differences between the new and other reddenings are found which are larger than about 2 sigma. The author had previously found that the M67 main-sequence stars have about the same blanketing as that of Coma and less blanketing than the Hyades; this conclusion is essentially unchanged by the revised reddenings

  19. Rapid fish stock depletion in previously unexploited seamounts: the ...

    African Journals Online (AJOL)

    Rapid fish stock depletion in previously unexploited seamounts: the case of Beryx splendens from the Sierra Leone Rise (Gulf of Guinea) ... A spectral analysis and red-noise spectra procedure (REDFIT) algorithm was used to identify the red-noise spectrum from the gaps in the observed time-series of catch per unit effort by ...

  20. 18 CFR 154.302 - Previously submitted material.

    Science.gov (United States)

    2010-04-01

    ... 18 Conservation of Power and Water Resources 1 2010-04-01 2010-04-01 false Previously submitted material. 154.302 Section 154.302 Conservation of Power and Water Resources FEDERAL ENERGY REGULATORY... concurrently with the rate change filing. There must be furnished to the Director, Office of Energy Market...

  1. The job satisfaction of principals of previously disadvantaged schools

    African Journals Online (AJOL)

    The aim of this study was to identify influences on the job satisfaction of previously disadvantaged school principals in North-West Province. Evans's theory of job satisfaction, morale and motivation was useful as a conceptual framework. A mixedmethods explanatory research design was important in discovering issues with ...

  2. Obstructive pulmonary disease in patients with previous tuberculosis ...

    African Journals Online (AJOL)

    Obstructive pulmonary disease in patients with previous tuberculosis: Pathophysiology of a community-based cohort. B.W. Allwood, R Gillespie, M Galperin-Aizenberg, M Bateman, H Olckers, L Taborda-Barata, G.L. Calligaro, Q Said-Hartley, R van Zyl-Smit, C.B. Cooper, E van Rikxoort, J Goldin, N Beyers, E.D. Bateman ...

  3. Abiraterone in metastatic prostate cancer without previous chemotherapy

    NARCIS (Netherlands)

    Ryan, Charles J.; Smith, Matthew R.; de Bono, Johann S.; Molina, Arturo; Logothetis, Christopher J.; de Souza, Paul; Fizazi, Karim; Mainwaring, Paul; Piulats, Josep M.; Ng, Siobhan; Carles, Joan; Mulders, Peter F. A.; Basch, Ethan; Small, Eric J.; Saad, Fred; Schrijvers, Dirk; van Poppel, Hendrik; Mukherjee, Som D.; Suttmann, Henrik; Gerritsen, Winald R.; Flaig, Thomas W.; George, Daniel J.; Yu, Evan Y.; Efstathiou, Eleni; Pantuck, Allan; Winquist, Eric; Higano, Celestia S.; Taplin, Mary-Ellen; Park, Youn; Kheoh, Thian; Griffin, Thomas; Scher, Howard I.; Rathkopf, Dana E.; Boyce, A.; Costello, A.; Davis, I.; Ganju, V.; Horvath, L.; Lynch, R.; Marx, G.; Parnis, F.; Shapiro, J.; Singhal, N.; Slancar, M.; van Hazel, G.; Wong, S.; Yip, D.; Carpentier, P.; Luyten, D.; de Reijke, T.

    2013-01-01

    Abiraterone acetate, an androgen biosynthesis inhibitor, improves overall survival in patients with metastatic castration-resistant prostate cancer after chemotherapy. We evaluated this agent in patients who had not received previous chemotherapy. In this double-blind study, we randomly assigned

  4. Response to health insurance by previously uninsured rural children.

    Science.gov (United States)

    Tilford, J M; Robbins, J M; Shema, S J; Farmer, F L

    1999-08-01

    To examine the healthcare utilization and costs of previously uninsured rural children. Four years of claims data from a school-based health insurance program located in the Mississippi Delta. All children who were not Medicaid-eligible or were uninsured, were eligible for limited benefits under the program. The 1987 National Medical Expenditure Survey (NMES) was used to compare utilization of services. The study represents a natural experiment in the provision of insurance benefits to a previously uninsured population. Premiums for the claims cost were set with little or no information on expected use of services. Claims from the insurer were used to form a panel data set. Mixed model logistic and linear regressions were estimated to determine the response to insurance for several categories of health services. The use of services increased over time and approached the level of utilization in the NMES. Conditional medical expenditures also increased over time. Actuarial estimates of claims cost greatly exceeded actual claims cost. The provision of a limited medical, dental, and optical benefit package cost approximately $20-$24 per member per month in claims paid. An important uncertainty in providing health insurance to previously uninsured populations is whether a pent-up demand exists for health services. Evidence of a pent-up demand for medical services was not supported in this study of rural school-age children. States considering partnerships with private insurers to implement the State Children's Health Insurance Program could lower premium costs by assembling basic data on previously uninsured children.

  5. Reoperative sentinel lymph node biopsy after previous mastectomy.

    Science.gov (United States)

    Karam, Amer; Stempel, Michelle; Cody, Hiram S; Port, Elisa R

    2008-10-01

    Sentinel lymph node (SLN) biopsy is the standard of care for axillary staging in breast cancer, but many clinical scenarios questioning the validity of SLN biopsy remain. Here we describe our experience with reoperative-SLN (re-SLN) biopsy after previous mastectomy. Review of the SLN database from September 1996 to December 2007 yielded 20 procedures done in the setting of previous mastectomy. SLN biopsy was performed using radioisotope with or without blue dye injection superior to the mastectomy incision, in the skin flap in all patients. In 17 of 20 patients (85%), re-SLN biopsy was performed for local or regional recurrence after mastectomy. Re-SLN biopsy was successful in 13 of 20 patients (65%) after previous mastectomy. Of the 13 patients, 2 had positive re-SLN, and completion axillary dissection was performed, with 1 having additional positive nodes. In the 11 patients with negative re-SLN, 2 patients underwent completion axillary dissection demonstrating additional negative nodes. One patient with a negative re-SLN experienced chest wall recurrence combined with axillary recurrence 11 months after re-SLN biopsy. All others remained free of local or axillary recurrence. Re-SLN biopsy was unsuccessful in 7 of 20 patients (35%). In three of seven patients, axillary dissection was performed, yielding positive nodes in two of the three. The remaining four of seven patients all had previous modified radical mastectomy, so underwent no additional axillary surgery. In this small series, re-SLN was successful after previous mastectomy, and this procedure may play some role when axillary staging is warranted after mastectomy.

  6. Upon Further Review: V. An Examination of Previous Lightcurve Analysis from the Palmer Divide Observatory

    Science.gov (United States)

    Warner, Brian D.

    2011-01-01

    Updated results are given for nine asteroids previously reported from the Palmer Divide Observatory (PDO). The original images were re-measured to obtain new data sets using the latest version of MPO Canopus photometry software, analysis tools, and revised techniques for linking multiple observing runs covering several days to several weeks. Results that were previously not reported or were moderately different were found for 1659 Punkajarju, 1719 Jens, 1987 Kaplan, 2105 Gudy, 2961 Katsurahama, 3285 Ruth Wolfe, 3447 Burckhalter, 7816 Hanoi, and (34817) 2000 SE116. This is one in a series of papers that will examine results obtained during the initial years of the asteroid lightcurve program at PDO.

  7. Estimation of the limit of detection with a bootstrap-derived standard error by a partly non-parametric approach. Application to HPLC drug assays

    DEFF Research Database (Denmark)

    Linnet, Kristian

    2005-01-01

    Bootstrap, HPLC, limit of blank, limit of detection, non-parametric statistics, type I and II errors......Bootstrap, HPLC, limit of blank, limit of detection, non-parametric statistics, type I and II errors...

  8. Determination of 9 Carcinogenic Dyes by HPLC-DAD%HPLC-DAD法检测染料产品中9种致癌染料

    Institute of Scientific and Technical Information of China (English)

    吕双; 季浩; 蒲爱军; 王勇

    2016-01-01

    本文建立了测定染料产品中9种致癌染料的高效液相色谱-二极管阵列检测器分析方法(HPLC-DAD).各类染料经溶解或萃取后,通过Symmetry Shield RP-18色谱柱分离后进入DAD检测器,采用外标法对9种致癌染料进行定性和定量分析.

  9. The metabolism of 4-bromoaniline in the bile-cannulated rat: application of ICPMS (79/81Br), HPLC-ICPMS & HPLC-oaTOFMS

    OpenAIRE

    Duckett, Catherine; McCullagh, Michael; Smith, Christopher; Wilson, Ian D

    2015-01-01

    ? 2015 The Author(s). Published by Taylor & Francis.1. An excretion balance study was performed following i.p. administration of 4-bromoaniline (50 mg kg-1) to bile-cannulated rats, using bromine-detected (79/81Br) ICPMS for quantification. Approximately 90% of the dose was recovered in urine (68.9 ? 3.6%) and bile (21.4 ? 1.4%) by 48 h post-administration.2. HPLC-ICPMS (79/81Br) was used to selectively detect and profile the major urinary and biliary-excreted metabolites and determined that ...

  10. Matched cohort study of external cephalic version in women with previous cesarean delivery.

    Science.gov (United States)

    Keepanasseril, Anish; Anand, Keerthana; Soundara Raghavan, Subrahmanian

    2017-07-01

    To evaluate the efficacy and safety of external cephalic version (ECV) among women with previous cesarean delivery. A retrospective study was conducted using data for women with previous cesarean delivery and breech presentation who underwent ECV at or after 36 weeks of pregnancy during 2011-2016. For every case, two multiparous women without previous cesarean delivery who underwent ECV and were matched for age and pregnancy duration were included. Characteristics and outcomes were compared between groups. ECV was successful for 32 (84.2%) of 38 women with previous cesarean delivery and 62 (81.6%) in the control group (P=0.728). Multivariate regression analysis confirmed that previous cesarean was not associated with ECV success (odds ratio 1.89, 95% confidence interval 0.19-18.47; P=0.244). Successful vaginal delivery after successful ECV was reported for 19 (59.4%) women in the previous cesarean delivery group and 52 (83.9%) in the control group (P<0.001). No ECV-associated complications occurred in women with previous cesarean delivery. To avoid a repeat cesarean delivery, ECV can be offered to women with breech presentation and previous cesarean delivery who are otherwise eligible for a trial of labor. © 2017 International Federation of Gynecology and Obstetrics.

  11. Glucosinolate diversity within a phylogenetic framework of the tribe Cardamineae (Brassicaceae) unraveled with HPLC-MS/MS and NMR-based analytical distinction of 70 desulfoglucosinolates.

    Science.gov (United States)

    Olsen, Carl Erik; Huang, Xiao-Chen; Hansen, Cecilie I C; Cipollini, Don; Ørgaard, Marian; Matthes, Annemarie; Geu-Flores, Fernando; Koch, Marcus A; Agerbirk, Niels

    2016-12-01

    As a basis for future investigations of evolutionary trajectories and biosynthetic mechanisms underlying variations in glucosinolate structures, we screened members of the crucifer tribe Cardamineae by HPLC-MS/MS, isolated and identified glucosinolates by NMR, searched the literature for previous data for the tribe, and collected HPLC-MS/MS data for nearly all glucosinolates known from the tribe as well as some related structures (70 in total). This is a considerable proportion of the approximately 142 currently documented natural glucosinolates. Calibration with authentic references allowed distinction (or elucidation) of isomers in many cases, such as distinction of β-hydroxyls, methylthios, methylsulfinyls and methylsulfonyls. A mechanism for fragmentation of secondary β-hydroxyls in MS was elucidated, and two novel glucosinolates were discovered: 2-hydroxy-3-methylpentylglucosinolate in roots of Cardamine pratensis and 2-hydroxy-8-(methylsulfinyl)octylglucosinolate in seeds of Rorippa amphibia. A large number of glucosinolates (ca. 54 with high structural certainty and a further 28 or more suggested from tandem MS), representing a wide structural variation, is documented from the tribe. This included glucosinolates apparently derived from Met, Phe, Trp, Val/Leu, Ile and higher homologues. Normal side chain elongation and side chain decoration by oxidation or methylation was observed, as well as rare abnormal side chain decoration (hydroxylation of aliphatics at the δ rather than β-position). Some species had diverse profiles, e.g. R. amphibia and C. pratensis (19 and 16 individual glucosinolates, respectively), comparable to total diversity in literature reports of Armoracia rusticana (17?), Barbarea vulgaris (20-24), and Rorippa indica (>20?). The ancestor or the tribe would appear to have used Trp, Met, and homoPhe as glucosinolate precursor amino acids, and to exhibit oxidation of thio to sulfinyl, formation of alkenyls, β-hydroxylation of aliphatic

  12. [Fatal amnioinfusion with previous choriocarcinoma in a parturient woman].

    Science.gov (United States)

    Hrgović, Z; Bukovic, D; Mrcela, M; Hrgović, I; Siebzehnrübl, E; Karelovic, D

    2004-04-01

    The case of 36-year-old tercipare is described who developed choriocharcinoma in a previous pregnancy. During the first term labour the patient developed cardiac arrest, so reanimation and sectio cesarea was performed. A male new-born was delivered in good condition, but even after intensive therapy and reanimation occurred death of parturient woman with picture of disseminate intravascular coagulopathia (DIK). On autopsy and on histology there was no sign of malignant disease, so it was not possible to connect previous choricarcinoma with amniotic fluid embolism. Maybe was place of choriocarcinoma "locus minoris resistentiae" which later resulted with failure in placentation what was hard to prove. On autopsy we found embolia of lung with a microthrombosis of terminal circulation with punctiformis bleeding in mucous, what stands for DIK.

  13. Challenging previous conceptions of vegetarianism and eating disorders.

    Science.gov (United States)

    Fisak, B; Peterson, R D; Tantleff-Dunn, S; Molnar, J M

    2006-12-01

    The purpose of this study was to replicate and expand upon previous research that has examined the potential association between vegetarianism and disordered eating. Limitations of previous research studies are addressed, including possible low reliability of measures of eating pathology within vegetarian samples, use of only a few dietary restraint measures, and a paucity of research examining potential differences in body image and food choice motives of vegetarians versus nonvegetarians. Two hundred and fifty-six college students completed a number of measures of eating pathology and body image, and a food choice motives questionnaire. Interestingly, no significant differences were found between vegetarians and nonvegetarians in measures of eating pathology or body image. However, significant differences in food choice motives were found. Implications for both researchers and clinicians are discussed.

  14. HPLC Quantification of astaxanthin and canthaxanthin in Salmonidae eggs.

    Science.gov (United States)

    Tzanova, Milena; Argirova, Mariana; Atanasov, Vasil

    2017-04-01

    Astaxanthin and canthaxanthin are naturally occurring antioxidants referred to as xanthophylls. They are used as food additives in fish farms to improve the organoleptic qualities of salmonid products and to prevent reproductive diseases. This study reports the development and single-laboratory validation of a rapid method for quantification of astaxanthin and canthaxanthin in eggs of rainbow trout (Oncorhynchus mykiss) and brook trout (Salvelinus fontinalis М.). An advantage of the proposed method is the perfect combination of selective extraction of the xanthophylls and analysis of the extract by high-performance liquid chromatography and photodiode array detection. The method validation was carried out in terms of linearity, accuracy, precision, recovery and limits of detection and quantification. The method was applied for simultaneous quantification of the two xanthophylls in eggs of rainbow trout and brook trout after their selective extraction. The results show that astaxanthin accumulations in salmonid fish eggs are larger than those of canthaxanthin. As the levels of these two xanthophylls affect fish fertility, this method can be used to improve the nutritional quality and to minimize the occurrence of the M74 syndrome in fish populations. Copyright © 2016 John Wiley & Sons, Ltd.

  15. Previous climatic alterations are caused by the sun

    International Nuclear Information System (INIS)

    Groenaas, Sigbjoern

    2003-01-01

    The article surveys the scientific results of previous research into the contribution of the sun to climatic alterations. The author concludes that there is evidence of eight cold periods after the last ice age and that the alterations largely were due to climate effects from the sun. However, these effects are only causing a fraction of the registered global warming. It is assumed that the human activities are contributing to the rest of the greenhouse effect

  16. Influence of previous knowledge in Torrance tests of creative thinking

    OpenAIRE

    Aranguren, María; Consejo Nacional de Investigaciones Científicas y Técnicas CONICET

    2015-01-01

    The aim of this work is to analyze the influence of study field, expertise and recreational activities participation in Torrance Tests of Creative Thinking (TTCT, 1974) performance. Several hypotheses were postulated to explore the possible effects of previous knowledge in TTCT verbal and TTCT figural university students’ outcomes. Participants in this study included 418 students from five study fields: Psychology;Philosophy and Literature, Music; Engineering; and Journalism and Advertisin...

  17. Analysis of previous screening examinations for patients with breast cancer

    International Nuclear Information System (INIS)

    Lee, Eun Hye; Cha, Joo Hee; Han, Dae Hee; Choi, Young Ho; Hwang, Ki Tae; Ryu, Dae Sik; Kwak, Jin Ho; Moon, Woo Kyung

    2007-01-01

    We wanted to improve the quality of subsequent screening by reviewing the previous screening of breast cancer patients. Twenty-four breast cancer patients who underwent previous screening were enrolled. All 24 took mammograms and 15 patients also took sonograms. We reviewed the screening retrospectively according to the BI-RADS criteria and we categorized the results into false negative, true negative, true positive and occult cancers. We also categorized the causes of false negative cancers into misperception, misinterpretation and technical factors and then we analyzed the attributing factors. Review of the previous screening revealed 66.7% (16/24) false negative, 25.0% (6/24) true negative, and 8.3% (2/24) true positive cancers. False negative cancers were caused by the mammogram in 56.3% (9/16) and by the sonogram in 43.7% (7/16). For the false negative cases, all of misperception were related with mammograms and this was attributed to dense breast, a lesion located at the edge of glandular tissue or the image, and findings seen on one view only. Almost all misinterpretations were related with sonograms and attributed to loose application of the final assessment. To improve the quality of breast screening, it is essential to overcome the main causes of false negative examinations, including misperception and misinterpretation. We need systematic education and strict application of final assessment categories of BI-RADS. For effective communication among physicians, it is also necessary to properly educate them about BI-RADS

  18. Study of HPLC/ICP-MS coupling for the As speciation; Estudo de um acoplamento de HPLC/ICP-MS para a especiacao do As

    Energy Technology Data Exchange (ETDEWEB)

    Cortez, Bruna C.G.; Oliveira, Arno Heeren de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: brunacortez2004@yahoo.com.br; heeren@nuclear.ufmg.br

    2005-07-01

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (As{sup III}) is more toxic than arsenate (As{sup V}). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  19. Quality Evaluation and Chemical Markers Screening of Salvia miltiorrhiza Bge. (Danshen Based on HPLC Fingerprints and HPLC-MSn Coupled with Chemometrics

    Directory of Open Access Journals (Sweden)

    Wenyi Liang

    2017-03-01

    Full Text Available Danshen, the dried root of Salvia miltiorrhiza Bge., is a widely used commercially available herbal drug, and unstable quality of different samples is a current issue. This study focused on a comprehensive and systematic method combining fingerprints and chemical identification with chemometrics for discrimination and quality assessment of Danshen samples. Twenty-five samples were analyzed by HPLC-PAD and HPLC-MSn. Forty-nine components were identified and characteristic fragmentation regularities were summarized for further interpretation of bioactive components. Chemometric analysis was employed to differentiate samples and clarify the quality differences of Danshen including hierarchical cluster analysis, principal component analysis, and partial least squares discriminant analysis. Consistent results were that the samples were divided into three categories which reflected the difference in quality of Danshen samples. By analyzing the reasons for sample classification, it was revealed that the processing method had a more obvious impact on sample classification than the geographical origin, it induced the different content of bioactive compounds and finally lead to different qualities. Cryptotanshinone, trijuganone B, and 15,16-dihydrotanshinone I were screened out as markers to distinguish samples by different processing methods. The developed strategy could provide a reference for evaluation and discrimination of other traditional herbal medicines.

  20. Chemical characterization of Azadirachta indica grafted on Melia azedarach and analyses of azadirachtin by HPLC-MS-MS (SRM) and meliatoxins by MALDI-MS.

    Science.gov (United States)

    Forim, Moacir Rossi; Cornélio, Vivian Estevam; da Silva, M Fátima das G F; Rodrigues-Filho, Edson; Fernandes, João B; Vieira, Paulo C; Matinez, Sueli Souza; Napolitano, Michael P; Yost, Richard A

    2010-01-01

    Melia azedarach adapted to cool climates was selected as rootstocks for vegetative propagation of Azadirachta indica. Cleft grafting of A. indica on M. azedarach rootstock showed excellent survival. Little is known about the chemistry of grafting. The roots, stems, leaves and seeds of this graft were examined in order to verify if grafted A. indica would produce limonoids different from those found in non-grafted plants. Intact matured fruits were also studied to verify if they were free of meliatoxins. After successive chromatographic separations the extracts afforded several limonoids. HPLC-MS/MS and MALDI-MS were used to develop sensitive methods for detecting azadirachtin on all aerial parts of this graft and meliatoxins in fruits, respectively. The stem afforded the limonoid salannin, which was previously found in the oil seeds of A. indica. Salannin is also found in the root bark of M. azedarach. Thus, the finding of salannin in this study suggests that it could have been translocated from the M. azedarach rootstock to the A. indica graft. HPLC-MS/MS analyses showed that azadirachtin was present in all parts of the fruits, stem, flowers and root, but absent in the leaves. The results of MALDI-MS analyses confirmed the absence of meliatoxins in graft fruits. This study showed that A. indica grafted onto M. azedarach rootstock produces azadirachtin, and also that its fruits are free of meliatoxins from rootstocks, confirming that this graft forms an excellent basis for breeding vigorous Neem trees in cooler regions.

  1. Structural investigations of flavonol glycosides from sea buckthorn (Hippophaë rhamnoides) pomace by NMR spectroscopy and HPLC-ESI-MS(n).

    Science.gov (United States)

    Rösch, Daniel; Krumbein, Angelika; Mügge, Clemens; Kroh, Lothar W

    2004-06-30

    Four flavonol glycosides were isolated from an extract of sea buckthorn pomace (Hippophaë rhamnoides) by Sephadex LH-20 gel chromatography and semipreparative HPLC. Their structures were elucidated by hydrolysis studies, ESI-MS(n), UV, and (1)H and (13)C NMR spectroscopy. The occurrence of the major flavonol glycoside kaempferol 3-O-beta-sophoroside-7-O-alpha-rhamnoside in sea buckthorn is described here for the first time. A further 21 flavonol glycosides of Sephadex LH-20 fractions of sea buckthorn pomace were characterized by HPLC-DAD-ESI-MS. The characteristic MS-MS and MS(3) fragmentation pattern of flavonol glycosides previously identified in sea buckthorn juice and of flavonol glycosides identified by NMR spectroscopy gave valuable indications for their identification. The results demonstrate that loss of the sugar moiety from C-7 of the aglycon is more favored than fission of the glycosidic linkage at the C-3 position. Thus, most of the compounds identified were 7-rhamnosides of isorhamnetin, kaempferol, and quercetin, which exhibit different substitution patterns at the C-3 position, mainly glucosides, rutinosides, and sophorosides. In addition, numerous flavonol glycosides were detected lacking a sugar moiety at C-7. Finally, eight flavonol derivatives were identified that are acylated by hydroxybenzoic or hydoxycinnamic acids.

  2. Clinical applications of HPLC-competitive protein binding assay for serum 25-hydroxyvitamin D

    Energy Technology Data Exchange (ETDEWEB)

    Shouli, Yang [China-Japan Friendship Hospital, Beijing, BJ (China). Inst. of Clinical Medical Science; and others

    1989-08-01

    This report describes the clinical applications of HPLC-competitive protein binding assay for serum 25(OH) Vit D in 156 cases. Serum 25(OH) Vit D of normal human was 33.1 +- 14.8 nmol/L (13.2 +- 5.9 ng/ml), while for various diseases are as follows: rickets, 18.0 +- 9.0 nmol/L (7.2 +- 3.6 ng/ml, n = 36, P < 0.005); hypervitaminosis D, 116.8 +- 31.3 nmol/L (46.7 +- 12.3 ng/ml, n = 6, P < 0.001); renal diseases of children, 25.3 +- 7.3 nmol/L (10.1 +- 2.9 ng/ml, n = 9. P > 0.1); pneumonia of children, 33.8 +- 14.8 nmol/L (13.5 +- 5.9 ng/ml, n = 10, P > 0.5); cirrhosis, 13.8 +- 11.3 nmol/L (5.5 +- 4.5 ng/ml, n = 9, P < 0.001); vasculitis, 25.5 +- 15.3 nmol/L (10.2 +- 6.1 ng/ml, n = 5, P > 0.2); administration of anticonvulsant (1 to 15 years), 19.0 +- 6.5 nmol/L (7.6 +- 2.6 ng/ml, n = 19, P < 0.001); administration of glococorticoids (> 6 months), 15.3 +- 5.0 nmol/L (6.1 +- 2.0 ng/ml, n = 6, P < 0.005); hyperthyroidism, 34.0 +- 23.5 nmol/L (13.6 +- 9.4 ng/ml, n = 13, P > 0.5); pregnant women, 39.8 +- 16.5 nmol/L (15.9 +- 6.6 ng/ml, n = 7, P > 0.1). We found it is a useful reference value for most of the above diseased state especially for differentiation between rickets and hypervitaminosis.

  3. Development and validation of an HPLC/UV/MS method for simultaneous determination of 18 preservatives in grapefruit seed extract.

    Science.gov (United States)

    Ganzera, Markus; Aberham, Anita; Stuppner, Hermann

    2006-05-31

    Grapefruit seed extracts are used in cosmetics, food supplements, and pesticides because of their antimicrobial properties, but suspicions about the true nature of the active compounds arose when synthetic disinfectants such as benzethonium or benzalkonium chloride were found in commercial products. The HPLC method presented herein allows the quality assessment (qualitative and quantitative) of these products for the first time. On the basis of a standard mixture of 18 preservatives most relevant for food and grapefruit products, a method was developed allowing the baseline separation of all compounds within 40 min. Optimum results were obtained with a C-8 stationary phase and a solvent system comprising aqueous trifluoroacetic acid, acetonitrile, and 2-propanol. The assay was fully validated and shown to be sensitive (LOD or = 96.1%), repeatable (sigma(rel) < or = 3.5%), precise (intra-day variation < or = 4.5%, interday variation < or = 4.1%), and rugged. Without any modifications the method could be adopted for LC-MS experiments, where the compounds of interest were directly assignable in positive ESI mode. The quantitative results of several products for ecofarming confirmed previous studies, as seven out of nine specimens were adulterated with preservatives in varying composition. The samples either contained benzethonium chloride (2.5-176.9 mg/mL) or benzalkonium chloride (138.2-236.3 mg/mL), together with smaller amounts of 4-hydroxybenzoic acid esters, benzoic acid, and salicylic acid.

  4. Detection of low plasma estradiol concentrations in nesting green turtles (Chelonia mydas) by HPLC/Ms-Ms.

    Science.gov (United States)

    Mahmoud, I Y; Alkindi, A Y; Khan, T; Al-Bahry, S N

    2011-03-01

    In previous studies on nesting green turtles under natural conditions from different geographical regions, 17-β-estradiol (E(2) ) was either undetectable or detected at very low levels. RIA and other related techniques were not sensitive enough to measure low E(2) values in the green turtles. In this study, a sensitive method was used in detecting low hormone concentrations: high performance liquid chromatography with tandem quadruple mass spectrometry (HPLC-MS/MS). Using this technique, estradiol for the first time was detected in nesting green turtles during the peak season (June-October) at Ras Al-Hadd Reserve, Oman. The E(2) values recorded from this study were the highest ever recorded from nesting green turtles in any geographical region, but the levels did not vary significantly throughout different phases of nesting. The presence of E(2) during nesting presumably plays a role in the physiology and behavior of this species. Ras Al-Hadd hosts one of the largest nesting populations of green turtles in the world, and an understanding of their nesting patterns may be of value in conservation and management programs for this endangered species. Copyright © 2011 Wiley-Liss, Inc., A Wiley Company.

  5. The pathogenicity of genetic variants previously associated with left ventricular non-compaction

    DEFF Research Database (Denmark)

    Abbasi, Yeganeh; Jabbari, Javad; Jabbari, Reza

    2016-01-01

    BACKGROUND: Left ventricular non-compaction (LVNC) is a rare cardiomyopathy. Many genetic variants have been associated with LVNC. However, the number of the previous LVNC-associated variants that are common in the background population remains unknown. The aim of this study was to provide...... an updated list of previously reported LVNC-associated variants with biologic description and investigate the prevalence of LVNC variants in healthy general population to find false-positive LVNC-associated variants. METHODS AND RESULTS: The Human Gene Mutation Database and PubMed were systematically...... searched to identify all previously reported LVNC-associated variants. Thereafter, the Exome Sequencing Project (ESP) and the Exome Aggregation Consortium (ExAC), that both represent the background population, was searched for all variants. Four in silico prediction tools were assessed to determine...

  6. Study of some physical aspects previous to design of an exponential experiment

    International Nuclear Information System (INIS)

    Caro, R.; Francisco, J. L. de

    1961-01-01

    This report presents the theoretical study of some physical aspects previous to the design of an exponential facility. The are: Fast and slow flux distribution in the multiplicative medium and in the thermal column, slowing down in the thermal column, geometrical distribution and minimum needed intensity of sources access channels and perturbations produced by possible variations in its position and intensity. (Author) 4 refs

  7. Possible pulmonary Rhizopus oryzae infection in a previously healthy child after a near-drowning incident.

    Science.gov (United States)

    Gerlach, Magdalena M; Lippmann, Norman; Kobelt, Louise; Petzold-Quinque, Stefanie; Ritter, Lutz; Kiess, Wieland; Siekmeyer, Manuela

    2016-06-01

    This article reports on a previously healthy 17-month-old boy who developed pulmonary mucormycosis after a near-drowning incident in a goose pond. The patient survived without neurological sequelae and recovered, under treatment with amphotericin B, from the rare and often invasive fungal infection with Rhizopus spp., usually occurring in immunodeficient patients.

  8. Reading Aloud: Does Previous Trial History Modulate the Joint Effects of Stimulus Quality and Word Frequency?

    Science.gov (United States)

    O'Malley, Shannon; Besner, Derek

    2013-01-01

    No one would argue with the proposition that how we process events in the world is strongly affected by our experience. Nonetheless, recent experience (e.g., from the previous trial) is typically not considered in the analysis of timed cognitive performance in the laboratory. Masson and Kliegl (2013) reported that, in the context of the lexical…

  9. Wolff-Parkinson-White syndrome with cleft lip and palate: A rare, previously unreported association

    Directory of Open Access Journals (Sweden)

    K Kannan

    2008-01-01

    Full Text Available Wolff-Parkinson-White syndrome, also called Pre Excitation Syndrome, is characterized by an extra pathway that conducts the electrical impulses from the atria to the ventricles without the normal delay. We are reporting a case of WPW syndrome with a cleft lip and palate, which is a rare association and previously unreported in literature.

  10. Previous Mental Disorders and Subsequent Onset of Chronic Back or Neck Pain : Findings From 19 Countries

    NARCIS (Netherlands)

    Viana, Maria Carmen; Lim, Carmen C W; Garcia Pereira, Flavia; Aguilar-Gaxiola, Sergio; Alonso, Jordi; Bruffaerts, Ronny; de Jonge, Peter; Caldas-de-Almeida, Jose Miguel; O'Neill, Siobhan; Stein, Dan J; Al-Hamzawi, Ali; Benjet, Corina; Cardoso, Graça; Florescu, Silvia; de Girolamo, Giovanni; Haro, Josep Maria; Hu, Chiyi; Kovess-Masfety, Viviane; Levinson, Daphna; Piazza, Marina; Posada-Villa, José; Rabczenko, Daniel; Kessler, Ronald C; Scott, Kate M

    Associations between depression/anxiety and pain are well established, but its directionality is not clear. We examined the associations between temporally previous mental disorders and subsequent self-reported chronic back/neck pain onset, and investigated the variation in the strength of

  11. Effects of previous growth hormone excess and current medical treatment for acromegaly on cognition

    NARCIS (Netherlands)

    Brummelman, Pauline; Koerts, Janneke; Dullaart, Robin P. F.; van den Berg, Gerrit; Tucha, Oliver; Wolffenbuttel, Bruce H. R.; van Beek, Andre P.

    2012-01-01

    Background In untreated acromegaly patients, decreased cognitive functioning is reported to be associated with the degree of growth hormone (GH) and IGF-1 excess. Whether previous GH excess or current medical treatment for acromegaly specifically affects cognition remains unclear. The aim of this

  12. Iodine-131 induced hepatotoxicity in previously healthy patients with Grave's disease.

    Science.gov (United States)

    Jhummon, Navina Priya; Tohooloo, Bhavna; Qu, Shen

    2013-01-01

    To describe the association of the rare and serious complication of liver toxicity in previously healthy Grave's disease (GD) patients after the treatment with radioactive iodine (131)I (RAI). We report the clinical, laboratory and pathologic findings of 2 cases of severe liver toxicity associated with the treatment with RAI in previously healthy patients with GD. Clinical examination and laboratory investigations excluded viral hepatitis, autoimmune hepatitis, granulomatous disease, primary biliary disease, extrahepatic biliary obstruction, and heart failure. Case 1: A previously healthy 52-years old man reportedly having a typical GD but following RAI treatment, concomitantly developed severe liver toxicity that required 1 week of treatment in hospital. Case 2: A previously healthy 34-years old woman is reported as having a typical GD but developed jaundice following RAI treatment that required several weeks of in hospital treatment in the hepato-biliary department. In both cases, the liver dysfunction resolved after intensive treatment with hepato-protective agents. In this report the therapeutic considerations as well as the pathogenetic possibilities are reviewed. To the best of our knowledge, this is the first description of the association observed, which is rare but may be severe and should be considered in any case of thyrotoxicosis where a liver dysfunction develops after the treatment with radioactive iodine (131)I.

  13. Iodine-131 induced hepatotoxicity in previously healthy patients with Grave’s disease

    Science.gov (United States)

    2013-01-01

    Objective To describe the association of the rare and serious complication of liver toxicity in previously healthy Grave’s disease (GD) patients after the treatment with radioactive iodine 131I (RAI). Case presentation We report the clinical, laboratory and pathologic findings of 2 cases of severe liver toxicity associated with the treatment with RAI in previously healthy patients with GD. Clinical examination and laboratory investigations excluded viral hepatitis, autoimmune hepatitis, granulomatous disease, primary biliary disease, extrahepatic biliary obstruction, and heart failure. Case 1: A previously healthy 52-years old man reportedly having a typical GD but following RAI treatment, concomitantly developed severe liver toxicity that required 1 week of treatment in hospital. Case 2: A previously healthy 34-years old woman is reported as having a typical GD but developed jaundice following RAI treatment that required several weeks of in hospital treatment in the hepato-biliary department. In both cases, the liver dysfunction resolved after intensive treatment with hepato-protective agents. In this report the therapeutic considerations as well as the pathogenetic possibilities are reviewed. Conclusion To the best of our knowledge, this is the first description of the association observed, which is rare but may be severe and should be considered in any case of thyrotoxicosis where a liver dysfunction develops after the treatment with radioactive iodine 131I. PMID:23497434

  14. Long-term effects of previous oxandrolone treatment in adult women with Turner syndrome

    NARCIS (Netherlands)

    Freriks, K.; Sas, T.C.J.; Traas, M.A.F.; Netea-Maier, R.T.; Heijer, M. den; Hermus, A.R.M.M.; Wit, J.M.; Alfen-van der Velden, J. van; Otten, B.J.; Muinck Keizer-Schrama, S.M.P.F. de; Gotthardt, M.; Dejonckere, P.H.; Zandwijken, G.R.; Menke, L.A.; Timmers, H.J.L.M.

    2013-01-01

    OBJECTIVE: Short stature is a prominent feature of Turner syndrome (TS), which is partially overcome by GH treatment. We have previously reported the results of a trial on the effect of oxandrolone (Ox) in girls with TS. Ox in a dose of 0.03 mg/kg per day (Ox 0.03) significantly increased adult

  15. Long-term effects of previous oxandrolone treatment in adult women with Turner syndrome

    NARCIS (Netherlands)

    K. Freriks (Kim); T.C.J. Sas (Theo); T. Traas (Theo); R.T. Netea-Maier (Romana ); M. den Heijer (Martin); A.R.M.M. Hermus (Ad); J.M. Wit (Jan); J.A.E.M. Van Alfen-van Der Velden (Janiëlle A. E.); B.J. Otten (Barto); S.M.P.F. de Muinck Keizer-Schrama (Sabine); M. Gotthardt (Martin); P.H. Dejonckere (Philippe); G.R.J. Zandwijken (Gladys); L.A. Menke (Leonie); H.J.L.M. Timmers

    2013-01-01

    textabstractObjective: Short stature is a prominent feature of Turner syndrome (TS), which is partially overcome by GH treatment. We have previously reported the results of a trial on the effect of oxandrolone (Ox) in girls with TS. Ox in a dose of 0.03 mg/kg per day (Ox 0.03) significantly

  16. Pulmonary carcinosarcoma initially presenting as invasive aspergillosis: a case report of previously unreported combination

    Directory of Open Access Journals (Sweden)

    Van Thien

    2010-01-01

    Full Text Available Abstract Carcinosarcoma of the lung is a malignant tumor composed of a mixture of carcinoma and sarcoma elements. The carcinomatous component is most commonly squamous followed by adenocarcinoma. The sarcomatous component commonly comprises the bulk of the tumor and shows poorly differentiated spindle cell features. Foci of differentiated sarcomatous elements such as chondrosarcoma and osteosarcoma may be seen. Aspergillus pneumonia is the most common form of invasive aspergillosis and occurs mainly in patients with malignancy, immunocompromizing or debilitating diseases. Patients with Aspergillus pneumonia present with fever, cough, chest pain and occasionally hemoptysis. Tissue examination is the most reliable method for diagnosis, and mortality rate is high. We describe a case of primary carcinosarcoma of the lung concurrently occurring with invasive pulmonary aspergillosis in a 66-year old patient.

  17. Non-detection of Previously Reported Transits of HD 97658b with MOST Photometry

    DEFF Research Database (Denmark)

    Dragomir, Diana; Matthews, Jaymie M.; Howard, Andrew W.

    2012-01-01

    The radial velocity-discovered exoplanet HD 97658b was recently announced to transit, with a derived planetary radius of 2.93 ± 0.28 R ⊕. As a transiting super-Earth orbiting a bright star, this planet would make an attractive candidate for additional observations, including studies of its atmosp...

  18. HPLC assay for 2-(3-aminopropylamino)ethanethiol (WR-1065) in plasma

    International Nuclear Information System (INIS)

    McGovern, E.P.; Swynnerton, N.F.; Steele, P.D.; Mangold, D.J.

    1984-01-01

    A high pressure liquid chromatography (HPLC) plasma assay for WR-1065 is described which is both precise and accurate throughout the concentration range from 1 to 500 μg/mL of plasma. The analyte is separated by HPLC and detected with a thiol specific electrochemical transducer cell. The detector response is linear over the ranges 1 to 10 μg/mL, 10 to 100 μg/mL, and 100 to 500 μg/mL. The absolute retention times for WR-1065 and WT-1729 are 9 and 12 minutes, respectively. The assay uses 100 μL of plasma and requires a total chromatography cycle time of 40 minutes. The method has been found suitable for the determination of WR-1065 in plasma from a beagle dog after i.v. administration of S-2-(3-aminopropylamino)ethyl phosphorothioate (WR-2721)

  19. Development of an HPLC post-column antioxidant assay for Solidago canadensis radical scavengers.

    Science.gov (United States)

    Marksa, Mindaugas; Radušienė, Jolita; Jakštas, Valdas; Ivanauskas, Liudas; Marksienė, Rūta

    2016-01-01

    The aim of this work was to modify and validate the post-column high-performance liquid chromatography (HPLC)-ABTS and DPPH methods for evaluating the antioxidant activity of the methanolic extracts of Solidago canadensis (Canadian goldenrod) leaves and flowers. Separation of the analytes was performed via the HPLC-PDA method on a YMC analytical column using a gradient elution program. Three compounds with antioxidant properties - chlorogenic acid, rutin and isoquercitrin - and two unidentified antioxidants were established. The research showed that the coil temperature regimes and loop length combinations influence the optimised post-column assay method for detecting the antioxidant activity of goldenrod radical scavengers. Investigations established that the temperature in the reaction coil was a substantial factor contributing to the signal strength of the analytes after reacting with the DPPH and ABTS radicals.

  20. Study of the electrooxidation of ethanol on hydrophobic electrodes by DEMS and HPLC

    International Nuclear Information System (INIS)

    Gonzalez Pereira, M.; Davila Jimenez, M.; Elizalde, M.P.; Manzo-Robledo, A.; Alonso-Vante, N.

    2004-01-01

    The electrochemical oxidation of ethanol in alkaline solution has been studied on Cu-PVC electrode and Ni/Cu-PVC composite electrodes modified by ruthenium nanoparticles. The techniques used were cyclic voltammetry (CV), steady-state potentiostatic method, on line differential electrochemical mass spectrometry (DEMS), and high-performance liquid chromatography (HPLC). The chemical products: acetaldehyde and acetic acid were detected measuring the proper mass charge (m/z) ratios. These products were also confirmed by HPLC. The surface modification of composite electrodes by ruthenium nanoparticles promotes the formation of acetaldehyde. As shown by DEMS, the surface modification shifts the onset potential for oxygen evolution reaction on the Cu-PVC composite electrode towards more anodic values

  1. Targeted natural product isolation guided by HPLC-SPE-NMR: Constituents of Hubertia species

    DEFF Research Database (Denmark)

    Sprogoe, K.; Staek, D.; Jager, A.K.

    2007-01-01

    -hydroxyphenyl)acetyl]quinic acid (3), was performed. Finally, targeted isolation of 1 was achieved by SPE fractionation and preparative HPLC, followed by evaluation of its antioxidant and antimicrobial activity. In contrast to chlorogenic acid and 3,5-di-O-caffeoylquinic acid, which act as antioxidants...... full or partial identification of all major extract constituents and demonstrated the presence of unusual quinic acid derivatives containing the (1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl residue that exhibit strongly coupled ABXY patterns, the parameters of which were obtained by spin simulations....... Using homo- and heteronuclear 2D NMR data acquired in the HPLC-SPE-NMR mode, complete structure determination of three new natural products, i.e., 3,5-di-O-caffeoyl-4-O-[(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl]quini c acid (1), its 2-hydroxy derivative (2), and 3,5-di-O-caffeoyl-4-O-[(4...

  2. Dual-mode gradient HPLC procedure for the simultaneous determination of chloroquine and proguanil.

    Science.gov (United States)

    Paci, A; Caire-Maurisier, A-M; Rieutord, A; Brion, F; Clair, P

    2002-01-01

    In order to assay the antipaludic capsule of the Service de Santé des Armées (SSA), that contains two antimalarial drugs, i.e. chloroquine sulfate (CQS, cp1) and proguanil hydrochloride (PGH, cp5), a HPLC procedure was developed. A reversed-phase ion-pair high-performance liquid chromatography (HPLC) method with an ultraviolet detection at 254 nm was set up and validated. Elution system includes programming of both organic concentration and flow-rate known as 'dual-mode gradient'. This method allows the simultaneous determination of both active compounds and separation of four process related substances. The method is simple, rapid, selective and accurate, and the precision is good with an inter- and intra-assay of <2%. The sensitivity is particularly suitable for pharmaceutical quality control.

  3. [Comparison between colorimetry and HPLC on the stability test of roxithromycin].

    Science.gov (United States)

    Wei, Z P; Mao, S R; Bi, D Z

    2000-11-01

    To compare the stability of roxithromycin in solutions of different pH. Roxithromycin solutions of different pH were prepared with water, simulate intestinal fluid (SIF) and simulate gastric fluid (SGF) shown to be the stability of these solutions were tested by colorimetry and HPLC. Roxithromycin was stable in water, SGF and SIF determined by colorimetry. However, it was found to be stable only in water and SIF but unstable in SGF as determined by HPLC. Roxithromycin is unstable in acidic medium like SGF. The metabolite of roxithromycin showed unfavorable interference on the assay of roxithromycin when colorimetry was used. Colorimetry can not be used for the determination and assay of roxithromycin in acidic solution like SGF.

  4. Stability Indicating RP-HPLC Method for Simultaneous Determination of Aspirin and Clopidrogel in Dosage Form

    International Nuclear Information System (INIS)

    Mohd Gousuddin; Sengupta, P.; Tripathi, V.D.; Das, A.

    2016-01-01

    Stability-indicating High Performance Liquid Chromatographic (HPLC) method was developed for simultaneous Aspirin and Clopidogrel, A Phenomenex Gemini C-18, 5 μm column having 250 mm x 4.6 mm i.d. in isocratic mode, with mobile phase containing buffer solution 0.3 % orthophosphoric acid : acetonitrile (65:35, v/v). The flow rate was 1 ml/ min and effluents were monitored at 266 nm. For linearity seven points calibration curve were obtained in a concentration range from 0.030-0.120 mg/ ml for aspirin and 0.015-0.060 mg/ ml for clopidogrel with correlation coefficient 0.9999. In the present study stability indicating HPLC method for the combination was tested by degrading the drugs together under various stress conditions like acid hydrolysis, base hydrolysis, oxidation, thermal and photolytic stress which is recommended by ICH guideline. (author)

  5. Simultaneous Determination of Lactulose and Lactose in Conserved Milk by HPLC-RID

    Directory of Open Access Journals (Sweden)

    Michelle Fernandes Silveira

    2015-01-01

    Full Text Available Heat treatment is applied to dairy products to ensure microbiological quality and increase the shelf life. However, a suitable control of this process is necessary to guarantee nutritional and sensory quality. The aim of this study is to adapt the high performance liquid chromatography (HPLC method for determination of lactulose and lactose content in commercial samples of UHT and sweetened condensed milk. The HPLC method used showed a good resolution of the analytes evaluated. The analyzed UHT milk samples presented levels for lactulose in accordance with the limit recommended by the International Dairy Federation. There was no significant variation in lactulose concentration for sweetened condensed milk samples. However, one sweetened condensed milk sample showed lactose level lower than the established values (10–12%.

  6. Authentication and distinction of Shenmai injection with HPLC fingerprint analysis assisted by pattern recognition techniques

    Directory of Open Access Journals (Sweden)

    Xue-Feng Lu

    2012-10-01

    Full Text Available In this paper, the feasibility and advantages of employing high performance liquid chromatographic (HPLC fingerprints combined with pattern recognition techniques for quality control of Shenmai injection were investigated and demonstrated. The Similarity Evaluation System was employed to evaluate the similarities of samples of Shenmai injection, and the HPLC generated chromatographic data were analyzed using hierarchical clustering analysis (HCA and soft independent modeling of class analogy (SIMCA. Consistent results were obtained to show that the authentic samples and the blended samples were successfully classified by SIMCA, which could be applied to accurate discrimination and quality control of Shenmai injection. Furthermore, samples could also be grouped in accordance with manufacturers. Our results revealed that the developed method has potential perspective for the original discrimination and quality control of Shenmai injection. Keywords: Shenmai injection, High performance liquid chromatography, Fingerprint, Pattern recognition

  7. HPLC based activity profiling for 5-lipoxygenase inhibitory activity in Isatis tinctoria leaf extracts.

    Science.gov (United States)

    Oberthür, C; Jäggi, R; Hamburger, M

    2005-06-01

    In the pursuit of the anti-inflammatory constituents in lipophilic woad extracts, the 5-lipoxygenase (5-LOX) inhibitory activity was investigated by HPLC-based activity profiling. In a low-resolution profiling, two time windows with peaks of activity were found. The first coincided with tryptanthrin, a known dual inhibitor of cyclooxygenase-2 (COX-2) and 5-LOX, whereas the major inhibitory fraction was towards the end of the HPLC run. The active fractions were profiled in a peak-resolved manner, and the compounds analyzed by LC-MS, GC and TLC. The activity in the lipophilic fractions of the Isatis extract could be linked to an unsaturated fatty acid, alpha-linolenic acid.

  8. Effective method for the detection of piroxicam in human plasma using HPLC.

    Science.gov (United States)

    Calvo, Adriana Maria; Prado, Mariel Tavares de Oliveira; Dionísio, Thiago José; Marques, Maria Paula; Brozoski, Daniel Thomas; Lanchote, Vera Lúcia; Faria, Flávio Augusto Cardoso; Santos, Carlos Ferreira

    2016-05-20

    Non-steroidal anti-inflammatory drugs (NSAIDs) are widely used by the general population to alleviate inflammation and pain after oral surgeries. Piroxicam is among the most commonly used NSAIDs and excels in controlling pain, swelling, trismus and other common symptoms of inflammation. This study aimed to evaluate different concentrations of piroxicam and its major metabolite, 5'-hydroxypiroxicam, in human plasma samples over time using high performance liquid chromatography (HPLC) after liquid-liquid extraction. Briefly, 10 volunteers participated in this study after approval by the Ethics Committee of Bauru School of Dentistry, Universidade de São Paulo - USP, Brazil. Volunteers received a single dose oral of piroxicam (20 mg) and had blood collected at various times following an established protocol. The methodology of liquid-liquid extraction was effective for determining concentrations of piroxicam in plasma using HPLC in 10 out of 10 volunteers while 5'-hydroxypiroxicam was only detected in 2 out of 10 volunteers.

  9. Separation of Alkyne Enantiomers by Chiral Column HPLC Analysis of Their Cobalt-Complexes

    Directory of Open Access Journals (Sweden)

    Qiaoyun Liu

    2017-03-01

    Full Text Available Separation of the enantiomers of new chiral alkynes in strategic syntheses and bioorthogonal studies is always problematic. The chiral column high-performance liquid chromatography (HPLC method in general could not be directly used to resolve such substrates, since the differentiation of the alkyne segment with the other alkane/alkene segment is not significant in the stationary phase, and the alkyne group is not a good UV chromophore. Usually, a pre-column derivatization reaction with a tedious workup procedure is needed. Making use of easily-prepared stable alkyne-cobalt-complexes, we developed a simple and general method by analyzing the in situ generated cobalt-complex of chiral alkynes using chiral column HPLC. This new method is especially suitable for the alkynes without chromophores and other derivable groups.

  10. Analysis of 2-ethylhexyl-p-methoxycinnamate in sunscreen products by HPLC and Raman spectroscopy.

    Science.gov (United States)

    Cheng, J; Li, Y S; L Roberts, R; Walker, G

    1997-10-01

    The analyses of 2-ethylhexyl-p-methoxycinnamate (EHMC) using HPLC and Raman spectroscopy have been undertaken and compared. EHMC, which is one of the most widely used sunscreen agents in suncare products in the US, exhibits a strong Raman signal. This signal clearly appears in both ethanol solutions of EHMC as well as in commercial sunscreen lotions containing this sun screen agent. A method for the direct detection and analysis of EHMC has been developed using Raman spectroscopy. This was accomplished by correlating the Raman intensities with the HPLC assays for a series of prototype suncare formulations. Based upon this information, it would be possible to employ Raman spectroscopy as an in-process control method in the commercial production of suncare products containing EHMC. The possibility of applying surface-enhanced Raman scattering for trace analysis was discussed.

  11. Experimental Studies of quantitative evaluation using HPLC and safety of Bee Venom Acupuncture

    Directory of Open Access Journals (Sweden)

    Seong Bong Jang

    2006-02-01

    Full Text Available Objectives : This study was conducted to carry out quantitative evaluation and safety of Bee Venom Acupuncture. Methods : Content analysis was done using HPLC, measurement of , and histological observations were made on the skin and muscles. Results : 1. According to HPLC analysis, each BVA-1 contained approximately , and BVA-2 contained approximately . But the volume of coating was so minute, slight difference exists between each needle. 2. LD50 of mouse with BVA-1 was 16 counts and this is equivalent to 640 needles/kg, making Bee Venom Acupuncture safe treatment apparatus. 3. Regardless of the number of needles, there was no sign of blood stasis or inflammation detected on the skin and muscle tissues. Conclusion : Above results indicate that the Bee Venom Acupuncture can complement shortcomings of syringe usage as a part of Oriental medicine treatment, but extensive researches should be done for further verification.

  12. Chromatographic characterization of 99mTc-EHDP complexes by HPLC and GPC

    International Nuclear Information System (INIS)

    Groot, G.J. de.

    1991-01-01

    Technetium-99m is a radioactive element and can be used in medical diagnostics. There are several technetium-99m complexes all having a specific preference for different organs. The aim of this thesis is to contribute to the identification of these complexes by analyzing them by the high performance liquid chromatography (HPLC) and the gel permeation chromatography (GPC) separation method. The first method separates with respect to the charge, the second one separates with respect to the size of the complexes. The HPLC method makes it possible to study the changes in the composition of the complex as a function of time. This kind of study is described in this thesis. Another part of this thesis describes the realization of a automated separation system. The advantages of the system compared to commercial available systems is that this system is less expensive and better suitable for measuring radioactive signals with a low intensity. (R.B.). 142 refs.; 30 figs.; 9 tabs

  13. Isolation and HPLC method development of azafrin from Alectra parasitica var. chitrakutensis.

    Science.gov (United States)

    Agrawal, Poonam; Laddha, Kirti; Tiwari, Ashok

    2014-01-01

    This study was undertaken to isolate and quantify azafrin in Alectra parasitica (Scrophulariaceae) rhizomes. A simple method for the isolation of carotenoid, azafrin, involves solvent extraction of the dried rhizome powder using a single solvent and further purification by recrystallisation. The structure of the compound was elucidated and confirmed by thin-layer chromatography, infrared spectroscopy, mass spectroscopy and nuclear magnetic resonance spectral analysis. A specific and rapid reversed-phase high-performance liquid chromatography (HPLC) method was developed for the analysis of azafrin. The method was validated for accuracy, precision, linearity and specificity. Validation revealed that the method is specific, accurate, precise, reliable and reproducible. The proposed HPLC method can be used for the identification and quantitative analysis of azafrin in A. parasitica rhizomes.

  14. Study of the electrooxidation of ethanol on hydrophobic electrodes by DEMS and HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez Pereira, M.; Davila Jimenez, M.; Elizalde, M.P.; Manzo-Robledo, A.; Alonso-Vante, N

    2004-09-15

    The electrochemical oxidation of ethanol in alkaline solution has been studied on Cu-PVC electrode and Ni/Cu-PVC composite electrodes modified by ruthenium nanoparticles. The techniques used were cyclic voltammetry (CV), steady-state potentiostatic method, on line differential electrochemical mass spectrometry (DEMS), and high-performance liquid chromatography (HPLC). The chemical products: acetaldehyde and acetic acid were detected measuring the proper mass charge (m/z) ratios. These products were also confirmed by HPLC. The surface modification of composite electrodes by ruthenium nanoparticles promotes the formation of acetaldehyde. As shown by DEMS, the surface modification shifts the onset potential for oxygen evolution reaction on the Cu-PVC composite electrode towards more anodic values.

  15. Discrimination of Black Ball-point Pen Inks by High Performance Liquid Chromatography (HPLC)

    International Nuclear Information System (INIS)

    Mohamed Izzharif Abdul Halim; Norashikin Saim; Rozita Osman; Halila Jasmani; Nurul Nadhirah Zainal Abidin

    2013-01-01

    In this study, thirteen types of black ball-point pen inks of three major brands were analyzed using high performance liquid chromatography (HPLC). Separation of the ink components was achieved using Bondapak C-18 column with gradient elution using water, ethanol and ethyl acetate. The chromatographic data obtained at wavelength 254.8 nm was analyzed using agglomerative hierarchical clustering (AHC) and principle component analysis (PCA). AHC was able to group the inks into three clusters. This result was supported by PCA, whereby distinct separation of the three different brands was achieved. Therefore, HPLC in combination with chemometric methods may be a valuable tool for the analysis of black ball-point pen inks for forensic purposes. (author)

  16. Automated injection of a radioactive sample for preparative HPLC with feedback control

    International Nuclear Information System (INIS)

    Iwata, Ren; Yamazaki, Shigeki

    1990-01-01

    The injection of a radioactive reaction mixture into a preparative HPLC column has been automated with computer control for rapid purification of routinely prepared positron emitting radiopharmaceuticals. Using pneumatic valves, a motor-driven pump and a liquid level sensor, two intelligent injection methods for the automation were compared with regard to efficient and rapid sample loading into a 2 mL loop of the 6-way valve. One, a precise but rather slow method, was demonstrated to be suitable for purification of 18 F-radiopharmaceuticals, while the other, due to its rapid operation, was more suitable for 11 C-radiopharmaceuticals. A sample volume of approx 0.5 mL can be injected onto a preparative HPLC column with over 90% efficiency with the present automated system. (author)

  17. [Determination of aristolochic acid A in Guanxinsuhe preparations by RP-HPLC].

    Science.gov (United States)

    Li, Lin; Gao, Hui-Min; Wang, Zhi-Min; Wang, Wei-Hao

    2006-01-01

    To establish a determination method of aristolochic acid A in Guanxisuhe preparations by RP-HPLC. The instrument used was Hewlett-Packard 1100 HPLC with a Alltech C18 column (4.6 mm x 250 mm, 5 microm). The mobile phase was methanol-water-acetic acid (68: 32:1) and the flow rate was 1.0 mL x min(-1). The UV detection wavelength was 390 nm and the column temperature was at 35 degrees C. The extracted solvent for the preparations was methanol solution contained 10% formic acid. The calibration curve was linear (r = 0.999 9) within the range of 0.119-1.89 microg for aristolochic acid A. The average recovery 99.0%, RSD 0.63%. The method with good linear relationship was convenient, quick, accurate, and suitable for the quality control of the aristolochic acid A in Guanxinsuhe and other traditional Chinese medicines containing aristolochic acid A.

  18. Analysis of D3-,4-,5-phosphorylated phosphoinositides using HPLC.

    Science.gov (United States)

    Munnik, Teun

    2013-01-01

    Detection of polyphosphoinositides (PPIs) is difficult due to their low chemical abundancy. This problem is further complicated by the fact that PPIs are present as various, distinct isomers, which are difficult, if not impossible, to separate by conventional thin layer chromatography (TLC) systems. PPIs in plants include PtdIns3P, PtdIns4P, PtdIns5P, PtdIns(3,5)P 2, and PtdIns(4,5)P 2. Here, a protocol is described analyzing plant PPIs using (32)P-orthophosphorus pre-labeled material. After extraction, lipids are deacylated and the resulting glycerophosphoinositol polyphosphates (GroPInsPs) separated by HPLC using a strong anion-exchange column and a shallow salt gradient. Alternatively, PPIs are first separated by TLC, the lipids reisolated, deacylated, and the GroPInsPs then separated by HPLC.

  19. [Simultaneous determination of eight kinds of conjunct bile acids in human bile by R-HPLC].

    Science.gov (United States)

    Dai, Z; Tan, G; Qian, K; Chen, X

    1997-01-01

    A method for the simultaneous determination of eight kinds of conjunct bile acids in human bile was developed by HPLC. They were separated on a YWG-C18 (3 microns) column at 30 degrees C, with methanol/water (65/35, V/V, pH3.0) as mobile phase, and detection wavelength at UV 210 nm. The linear ranges were 50-1,000 microns.ml-1, the recoveries were 91.2%-108.6%. The biles of 30 cases with cholelithiasis cholecystolithiasis and 20 cases without gallstone were detected by HPLC. The results showed that the constitution of bile acids was different between patients with cholelithiasis cholecystolithiasis and patients without gallstone.

  20. Development of Hplc Techniques for the Analysis of Trace Metal Species in the Primary Coolant of a Pressurised Water Reactor.

    Science.gov (United States)

    Barron, Keiron Robert Philip

    Available from UMI in association with The British Library. The need to monitor corrosion products in the primary circuit of a pressurised water reactor (PWR), at a concentration of 10pg ml^{-1} is discussed. A review of trace and ultra-trace metal analysis, relevant to the specific requirements imposed by primary coolant chemistry, indicated that high performance liquid chromatography (HPLC), coupled with preconcentration of sample was an ideal technique. A HPLC system was developed to determine trace metal species in simulated PWR primary coolant. In order to achieve the desired detection limit an on-line preconcentration system had to be developed. Separations were performed on Aminex A9 and Benson BC-X10 analytical columns. Detection was by post column reaction with Eriochrome Black T and Calmagite Linear calibrations of 2.5-100ng of cobalt (the main species of interest), were achieved using up to 200ml samples. The detection limit for a 200ml sample was 10pg ml^{-1}. In order to achieve the desired aim of on-line collection of species at 300^circ C, the use of inorganic ion-exchangers is essential. A novel application, utilising the attractive features of the inorganic ion-exchangers titanium dioxide, zirconium dioxide, zirconium arsenophosphate and pore controlled glass beads, was developed for the preconcentration of trace metal species at temperature and pressure. The performance of these exchangers, at ambient and 300^ circC was assessed by their inclusion in the developed analytical system and by the use of radioisotopes. The particular emphasis during the development has been upon accuracy, reproducibility of recovery, stability of reagents and system contamination, studied by the use of radioisotopes and response to post column reagents. This study in conjunction with work carried out at Winfrith, resulted in a monitoring system that could follow changes in coolant chemistry, on deposition and release of metal species in simulated PWR water loops. On