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Determination of gemcitabine and its metabolite in human plasma using high-pressure liquid chromatography coupled with a diode array detector

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Acta Pharmacologica Sinica 2004年第12期25卷 18-23页

作者： Neng-ming LIN2,3, Su ZENG2,4, Sheng-lin MA3, Yun FAN3, Hai-jun ZHONG3, Luo FANG3 2Collegeof Pharmaceutical Sciences, Zhejiang University, Hangzhou 310031 3Zhejiang Cancer Hospital, Hangzhou 310022, China College of Pharmaceutical Sciences Zhejiang University Hangzhou 310031 Zhejiang Cancer Hospital Hangzhou 310022

AIM: To establish a high pressure liquid chromatography (HPLC) method for determination of the concentration of gemcitabine (dFdC) and its metabolite(dFdU) in human plasma. METHODS: Plasma 1.0 mL spikedwith floxuridine as an internal standard was extracted with 3.0 mL of methanol-acetonitrile (v/v, 1:9). The supernatant was evapo- rated at 60 oC and the residue was reconstituted with 0.5 mL of the solution used as the mobile phase. After centrifugation, 50 μL of the supernatant was injected into the HPLC system. Separation was achieved on a C18 (4.6 mm×250 mm, 5 μm) column at 25 oC with the flow rate of the mobile phase set to 0.8 mL/min. The compounds were detected at 268 nm. The mobile phase consisted of 40.0 mmol/L acetate ammonium buffer solution (pH 5.5) and acetonitrile (v/v, 97.5:2.5). RESULTS: The linear range was 0.20-10.0 mg/L(r=0.9999) for dFdC and 0.50-50.0 mg/L(r=0.9999) for dFdU. The limit of detection (LOD) was 0.10 mg/L for dFdC and 0.25 mg/L for dFdU, while the limit of quantification (LOQ) was 0.20 mg/L (RSD<10 %) for dFdC and 0.50 mg/L(RSD <3 %) for dFdU. The average recovery of dFdC and dFdU by this method were 103.3 % and 98.7 %, respectively. For intra-day and inter-day, the corresponding standard deviations of the measurements of dFdC and dFdU were both less than 5.5 %. CONCLUSION: An analytical method was established to measure the concentrations of dFdC and dFdU in human plasma and was effectively applied to the dFdC and dFdU pharmacokinetic studies of 8 Chinese patients with malignant tumors.

关键词： high pressure liquid chromatography gemcitabine deoxycytidine floxuridine

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Analysis of Pesticide Raid^(█) in Feed of Wistar Rat by high-pressure liquid chromatography (HPLC)

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American Journal of Analytical Chemistry 2011年第8期2卷 32-36页

作者： Albert C. Achudume Institute of Ecology and Environmental Studies Obafemi Awolowo UniversityIle-IfeNigeria

The distribution of pesticide by-product in tissues of wistar rats were analyzed using high pressure liquid chromatography. The limit of detection of the HPLC was 0.1 μg. Results show bioaccumulation factor of pesticide “Raid?” in lipid, up to three times that of the feed at the first concentration and gradually decreased as the concentration increased in the muscle > (0.7), brain > (0.5) and liver > (0.3) as indicated in the text. At higher concentration of 961 μg/g, bioaccumulation factor decreased in the lipid to 1.2 and 0.6 in the muscle, 0.03 in the brain and 0.08 in the liver respectively. high pressure liquid chromatography (HPLC) analysis of raid extract suggests the presence of micprothrin and palethrin. The implications are numerous, but simply put that accidental ingestion of chlorinated hydrocarbon as in “Raid?” may involve convulsions, collapse and coma after only brief excitation and ataxia at the onset.

关键词： high pressure liquid chromatography Pesticide Raid^(█) Chlorinated Hydrocarbon Bioaccumulation

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Quantitative Single-Ion Irradiation by ASIPP Microbeam

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Chinese Physics Letters 2004年第5期21卷 821-824页

作者：王旭飞陈连运胡智文王晓华张俊李军陈斌胡素华时钟涛吴瑜许明亮吴李君王绍虎余增亮 KeyLaboratoryofIonBeamBioengineering ChineseAcademyofSciencesHefei230031

A single-ion microbeam facility has been constructed by the microbeam research group in ASIPP (Institute of Plasma Physics, Chinese Academy of Science). The system was designed to deliver defined numbers of hydrogen ions produced by a van de Graaff accelerator, covering an energy range from 200 keV to 3 MeV, into living cells (5 μm –20 μm diameter) growing in culture on thin plastic films. The beam is collimated by a 1-μm inner diameter HPLC (high performance liquid chromatography) capillary, which forms the micron-dimensional beam-line exit. A microbeam collimator, a scintillation ion counting system and a fast beam shutter, which constitute a precise dosage measuring and controlling system, jointly perform quantitative single-ion irradiation. With this facility, we can presently acquire ion-hitting efficiency close to 95%.

关键词： ion irradiation hydrogen ions ENERGY RANGE counting system Plasma physics Chrysanthemum morifolium control systems Academies of science Irradiation Van de Graaff accelerators high pressure liquid chromatography

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Contents of four active components in different commercial crude drugs and preparations of Danshen (Salvia miltiorrhiza)

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Acta Pharmacologica Sinica 2002年第12期23卷 110-115页

作者： Susan Wai Sum LEUNG,Yaw Loong SIOW,Ricky Ying Keung MAN Department of Pharmacology Faculty of Medicine University of Hong Kong 21 Sassoon Road Hong Kong China Department of Pharmacology Faculty of Medicine University of Hong Kong 21 Sassoon Road Hong Kong China Department of Pharmacology Faculty of Medicine University of Hong Kong 21 Sassoon Road Hong Kong China Department of Pharmacology University of Hong Kong 21 Sassoon Road Hong Kong China

AIM: To detect the contents of four active components of Salvia miltiorrhiza in various commercially available danshen crude drugs and preparations. METHODS: Commercially available danshen crude drugs from different sources, as well as danshen pills and intravenous injection preparations containing danshen alone or in combination with other herbs were collected. The composition of these danshen samples was analyzed using HPLC. Specifically, the amounts of magnesium tanshinoate B (MTB), danshensu, isotanshinone IIA, and ctyptotanshinone were determined. In some of these samples, the content of MTB was further confirmed by liquid chromatography-tandem mass spectrometer (LC-MS)/MS method. RESULTS: There were great variations in the amount of the four active ingredients in the commercially available danshen crude drugs and drug preparations in this study. The amount of MTB was the highest among the four components measured in the crude drugs. However, the amounts of MTB in all danshen preparations were much

关键词： Salvia miltiorrhiza magnesium tanshinoate B (MTB) high pressure liquid chromatography

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Clinical and genetic characteristics of Chinese hereditary nonpolyposis colorectal cancer families

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World Journal of Gastroenterology 2006年第25期12卷 4074-4077页

作者： Xu-Lin Wang Ying Yuan Su-Zhan Zhang Shan-Rong Cai Yan-Qin Huang Qiang Jiang Shu Zheng Cancer Institute the 2nd Affiliated Hospital College of Medicine Zhejiang University 88 Jie-Fang Road Hangzhou 310009 Zhejiang Province China

AIM： To analyze the clinical characteristics of Chinese hereditary nonpolyposis colorectal cancer （HNPCC） families and to screen the germline mutations of human mismatch repair genes hMLH1 and hMSH2 in the probands. METHODS： Thirty-one independent Chinese HNPCC families were collected in Zhejiang Province. All of them met Chinese HNPCC criteria. Clinical data about patient gender, site of colorectal cancer, age of onset, history of multiple colorectal cancer, associated extracolonic cancer were recorded. PCR and denaturing high performance liquid chromatography （DHPLC） were employed to screen the mutations. Sequencing analysis was used to find out the exact mutation site and characteristics of the samples showing abnormal DHPLC profiles. RESULTS： One hundred and thirty-six malignant neoplasms were found in 107 patients including 14 multiple cancers. One hundred and six of the 136 neoplasms （77.9%） were diagnosed as colorectal cancer, with an average age of onset at 48.57 ±29.00 years. Gastric cancer was the most common extracolonic cancer （10.3%） in these families. Twenty-three different sequence variations in hMLHI and hMSH2 genes were detected in these 17 families. Fifteen sequence variations were located in the exons, including 5 SNPs, 3 silent mutations, 3 missense mutations, 2 nonsense mutations and 2 frameshift mutations. The latter seven mutations seemed to be pathogenic. CONCLUSION： Germline mutations of hMLH1 and hMSH2 genes are identified in about one-third HNPCC kindreds fulfilling Chinese HNPCC criteria. Chinese HNPCC families have some particular clinical characteristics, such as a left-sided predominance, less synchronous or metachronous colorectal cancer, and frequent occurrence of gastric cancer.

关键词： Colorectal cancer Hereditary nonpolyposis DNA mutation analysis high pressure liquid chromatography Oncogenes

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Pharmacokinetics of CPU0213,a novel endothelin receptor antagonist,after intravenous administration in mice

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Acta Pharmacologica Sinica 2006年第3期27卷 367-371页

作者： Li GUAN~2 Yu FENG~2 Min JI~4 De-zai DAI~(2,3) ~2Research Division of Pharmacology,and ~4Center of New Drug Research and Development.China Pharmaceutical University,Nanjing 210009.China ResearchDivisionofPharmacology ChinaPharmaceuticalUniversityNanjing210009China CenterofNewDrugResearchandDevelopment.ChinaPharmaceuticalUniversity Nanjing210009China

Aim:To determine the pharmacokinetics associated with acute toxic doses ofCPU0213,a novel endothelin receptor antagonist in mice after a single intrave-nous ***:Concentrations in serum and the pharmacokineticparameters of CPU0213 were assayed by high pressure liquid chromatography(HPLC)following a single intravenous bolus of CPU0213 at concentrations of 25,50,and 100 mg/kg in *** intravenous acute toxicity of CPU0213 was alsoassessed in ***:A simple,sensitive and selective HPLC method wasdeveloped for quantitative determination of CPU0213 in mouse *** con-centration-time data conform to a 2-compartment model after iv administration ofCPU0213 at concentrations of 25,50,100 mg/*** corresponding distributionhalf-lives(T1/2α) were 3.6,4.2,1.1 min and the elimination half-lives(T1/2β)were39.4,70.3,61.9 *** was a linear increase in C0proportional to dose,and thesame as AUC0-tand AUC0-∞.AUC0-tand AUC0-∞were 4.511,13.070,23.666 g·min·L-1and 4.596,13.679,24.115 g·min·L-1,*** intravenous LD50was 315.5mg/***:First order rate pharmacokinetics were observed for CPU0213within the range of doses used,and the acute toxicity of CPU0213 is mild.

关键词： CPU0213 high pressure liquid chromatography mice pharmacokinetics acute toxicity

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Effect of oral administration of vitamin C on human aqueous humor ascorbate concentration

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中国药理学报 1999年第10期20卷 879-883页

作者： Zafar IQBAL John M MIDGLEY David G WATSON Stilianous D KARDITSAS Gordon N DUTTON William S WILSON Department of Pharmacy University of StrathclydeGlasgow G11XWUK Tennent Institute of Ophthalmology Western InfirmaryGtasgowG116NTUK Department of Pharmacology University of GlasgowGlasgow G128QQUK

AIM:To study oral administration of vitamin C on human aqueous humour ascorbate ***:high performance liquid chromatography(HPLC)coupled with electrochemical detector(BCD)was *** effect of oral administration of various doses of ascorbic acid,0(control),1.0,1.5,2.0,3.0,and 5.0 g,on its concentration in aqueous humour,obtained from volunteer cataract patients was ***:The concentration of ascorbic acid in aqueous humour of control group without administration of vitamin-C tablet or drug containing ascorbic acid was(254±119)mg·L^(-1).This study revealed that the administration of 2.0 g *** acid saturate the aqueous humour and further increase in the dose(3.0 g and 5.0 g)did not increase its concentration in aqueous humour,although its concentration was increased in ***:Oral administration of 2.0 g of Vc is sufficient to saturate the aqueous humour where it may be helpful in controlling the intra-ocular pressure.

关键词： aqueous humour ascorbic acid plasma cataract extraction high pressure liquid chromatography hydroquinones

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Analysis of Hupehenine in the Total Alkaloids from Fritillaria hupehensis by HPLC-ELSD

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Journal of Huazhong University of Science and Technology(Medical Sciences) 2008年第1期28卷 118-120页

作者：张鹏李娟张国欣皮慧芳张勇慧阮汉利吴继洲 Faculty of Pharmaceutical Sciences Tongji Medical College Huazhong University of Science and Technology

A reverse-phase high pressure liquid chromatography （HPLC） method with evaporative light scattering detection （ELSD） has been developed for the quantitative analysis of hupehenine in the total alkaloids from Fritillaria hupehensis. Samples were analyzed on a reverse-phase column （Hypersil C-18） with a mobile phase of methanol：water：chloroform： triethylamine （85：15：1：0.6）. The ELSD was set at the drift tube temperature of 68.3℃ and gas flow rate of 1.8 L/min. Hupehenine＇s retention time was 13.7 min with an asymmetry factor of 1.2. The validity of the method has been verified with linearity, limit of detection, accuracy and precision. The logarithmic linear curve was obtained from 8.936 to 134.04 μg/mL （r=0.9993）. The detection limit （S/N〉3） of hupehenine was 1.79 μg/mL on the column. Intra-day RSD was 1.42% and inter-day RSD was 2.26% （3 days within a week）. The average recovery of hupehenine was 101.50%, and RSD was 1.62%.

关键词： Fritillaria hupehensis the total alkaloids hupehenine high pressure liquid chromatography evaporative light scattering detection

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Effect of combination of extracts of ginseng and ginkgo biloba on acetylcholine in amyloid beta-protein-treated rats determined by an improved HPLC

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Acta Pharmacologica Sinica 2004年第9期 16-21页

作者： Jian-xun LIU, Wei-hong CONG, Li XU, Jian-nong WANG Research Center, Xiyuan Hospital, China Academy of Traditional Chinese Medicine, Beijing 100091, China

AIM: To determine the concentration of acetylcholine (ACh) in amyloid beta-protein (Aβ) treated rats and offer a method determining ACh as well. METHODS: A 1-month combination of extrats of ginseng and ginkgo biloba (Naoweikang) ig administration to rats was performed daily after bilateral injection of Aβ1-40 (4 g/L, 1μL for each side) into hippocampus. After

关键词： ginseng ginkgo biloba acetylcholine high pressure liquid chromatography amyloid beta-protein

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In vitro identification of metabolites of verapamil in rat liver microsomes

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Acta Pharmacologica Sinica 2004年第1期 123-130页

作者： Lu SUN, Shu-qiu ZHANG, Da-fang ZHONG Laboratory of Drug Metabolism and Pharmacokinetics, Shenyang Pharmaceutical University, Shenyang 110016, China

AIM: To investigate the metabolism of verapamil at low concentrations in rat liver microsomes. METHODS: Liver microsomes of Wistar rats were prepared using ultracentrifuge method. The in vitro metabolism of verapamil was studied with the rat liver microsomal incubation at concentration of 1.0 μmol/L and 5.0 umol/L. The metabolites were separated and assayed by liquid chromatography-ion trap mass

关键词： verapamil in vitro metabolism liver microsomes high pressure liquid chromatography mass spectrometry

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