共查询到20条相似文献,搜索用时 15 毫秒
1.
N. V. S. Ramakrishna K. N. Vishwottam S. Manoj M. Koteshwara M. Santosh Y. Anjaneyulu 《Chromatographia》2006,63(3-4):135-141
A simple, rapid, sensitive and selective liquid chromatography / tandem mass spectrometry method was developed and validated
for the quantification of pentoxifylline, a haemorheological agent. The analyte and internal standard, tamsulosin were extracted
by liquid-liquid extraction with ethyl acetate and were separated using an isocratic mobile phase on a reverse phase C18 column. The analytes were analyzed by mass spectrometry in the multiple reaction monitoring mode using the respective [M+H]+ ions, m/z 279/138 for pentoxifylline and m/z 409/228 for the IS. The assay exhibited a linear dynamic range of 2–1000 ng
mL−1 for pentoxifylline in human plasma. The lower limit of quantification was 2 ng mL−1 with a relative standard deviation of less than 10%. Acceptable precision and accuracy were obtained for concentrations over
the standard curve range. A run time of 1.5 min for each sample made it possible to analyze more than 400 human plasma samples
per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic,
bioavailability or bioequivalence studies.
Revised: 4 and 20 October 2005 相似文献
2.
建立了测定人血浆中卡托普利的LC/MS/MS法。取血浆0.2 mL,用对溴苯甲酰甲基溴进行衍生化,经甲醇沉淀蛋白后,以甲醇-10 mmol/L乙酸铵-甲酸(80/20/0.4,V/V)为流动相,用Zorbax SB-C18柱分离,通过配有电喷雾离子化源的四极杆-线性离子阱质谱仪,以多反应监测(MRM)方式进行检测。用于定量分析的离子反应分别为m/z416→m/z216(卡托普利衍生物)和m/z28→m/z193(安定)。卡托普利的线性范围为2.5~1000μg/L,最低定量限为2.5μg/L,样品分析时间为2.0 m in。该法精密、准确,在灵敏度和分析速度上优于以往文献报道,适用于游离型卡托普利血药浓度的监测和药动学研究。 相似文献
3.
Quantification of Clenbuterol in Human Plasma and Urine by Liquid Chromatography-Tandem Mass Spectrometry 总被引:1,自引:0,他引:1
The quantitative determination of clenbuterol in human plasma and urine is of particular interest for various fields such
as clinical and forensic research and doping controls. A simple and rapid sample preparation procedure based on liquid-liquid
extraction with subsequent re-extraction followed by liquid chromatography and electrospray ionization tandem mass spectrometry
allowed the determination of clenbuterol in urine and plasma at detection and quantification limits of 0.1 ng mL−1 and 0.2 ng mL−1, respectively, with recoveries ranging from 85–96%. The fast and robust nature of the assay provides a rapid and cost-effective
alternative to established procedures utilizing solid-phase extraction strategies. 相似文献
4.
Turbulent flow chromatography coupled to tandem mass spectrometry (TFC-MS-MS) has been widely used within bioanalysis, because of the ability to inject directly neat biological samples with no prior pretreatment. TFC-MS-MS removes the need for time consuming sample preparation procedures such as protein precipitation, liquid-liquid extraction or solid-phase extraction. There are two standard configurations that are commonly adopted for the use of TFC, namely fast elute and focus mode. In this paper, a new micro TFC column which has the advantages of reducing solvent consumption and improving mass sensitivity, was used to develop a fast elute method. A wide range of pharmaceutical compounds with various physicochemical properties was used to assess the system performance. Carry-over has often been identified as a potential source of inaccuracy in a fast elute mode. This paper shows how by using a systematic approach, carryover was eliminated. The parameters influencing the robustness of the micro TFC column are also discussed. This method was fully validated for a Pfizer development compound in human plasma using a new TFC parallel platform allowing two systems to be operated in parallel. Multiplexing the sample analysis allowed a 2-fold increase in throughput and provided an efficient use of the mass spectrometer. 相似文献
5.
A. Lakshmi Sailaja K. Kishore Kumar D. V. R. Ravi Kumar C. Mohan Kumar N. M. Yugandhar G. Srinubabu 《Chromatographia》2007,65(5-6):359-361
A simple, rapid, and sensitive high-performance liquid chromatographic method for estimation of efavirenz in human plasma
has been developed and validated. Chromatography was performed with C18 analytical column and 50:50 acetonitrile–phosphate buffer (pH 3.5) as mobile phase. Compounds were monitored by UV detection
at 247 nm. The retention time for efavirenz was 6.45 min and that for the internal standard, nelfinavir, was 2.042 min. Response
was a linear over the concentration range of 0.1 μg–10 μg mL−1 in human plasma. The method was simple, specific, precise and accurate and was useful for bioequivalence and pharmacokinetic
studies of efavirenz. 相似文献
6.
Kibum Kim Haehum Jung Hyi-Yoel Yun Seung-Ok Moon Young-Ran Yoon Kwang-il Kwon Hyesoo Kim Soojung Shon Wonku Kang 《Chromatographia》2007,66(3-4):257-260
The purpose of this investigation was to develop a method for measuring the concentration of octylonium in human plasma. Hydrochloric
acid was added to the plasma samples before pretreatment to improve the stability of the octylonium. After liquid–liquid extraction
with ethylacetate and isopropanol (10:1), the analytes were separated by chromatography on a reversed-phase C18 column and detected by LC–MS–MS with electrospray ionization–ionization. The coefficient of variation for the precision of
the assay was less than 10.1%, and the accuracy ranged from 98.0 to 106.5%. The limit of quantification or sensitivity was
0.2 ng mL−1. This method was validated by measuring octylonium in the plasma of healthy human subjects after administration of a single
120-mg oral dose of octylonium bromide. Thus, a highly sensitive and accurate analytical method was developed to determine
the concentration of octylonium in human plasma. 相似文献
7.
为评价盐酸头孢替安酯片在健康人体内的药代动力学特征,应用蛋白沉淀-液相色谱-串联质谱技术建立了灵敏度高、特异性强、快速的健康受试者血浆中头孢替安的分析方法。选用 Waters Symmtry C18色谱柱(50 mm×4.6 mm,5μm),以甲醇和1 mmol/ L 乙酸铵水溶液梯度洗脱,流速1.0 mL/ min。在多反应监测模式(MRM)下,采用电喷雾离子化源,正离子扫描模式下进行定量分析。标准曲线在5.0~5000 ng/ mL 范围内线性关系良好(r>0.99),定量下限为5.0 ng/ mL,方法学验证部分结果均符合生物样本定量测定的要求。本方法快速、灵敏、重现性好,并成功应用于健康受试者盐酸头孢替安酯片药动学研究,同时也为同类药物在人体生物基质中的定量检测提供参考。 相似文献
8.
Ahmed M. Abdel-Megied Wagdy M. Eldehna Mohamed A. Abdelrahman Fawzy A. Elbarbry 《Molecules (Basel, Switzerland)》2020,25(23)
In the present study, a sensitive and fully validated bioanalytical high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the quantitative determination of three newly synthesized carbonic anhydrases inhibitors (CAIs) with potential antitumor activity in human plasma. The analytes and the internal standard (IS) were extracted using 1.5 mL acetonitrile from only 450 µL aliquots of human plasma to achieve the desired protein precipitation. Chromatographic separations were achieved on Phenomenex Kinetex® C18 column (100 × 4.6 mm, 2.6 µm) using a binary gradient elution mode with a run time of less than 6 min. The mobile phase consisted of solvent (A): 0.1% formic acid in 50% methanol and solvent B: 0.1% formic acid in acetonitrile (30:70, v/v), pumped at a flow rate of 0.8 mL/min. Detection was employed using triple quadrupole tandem mass spectrometer (API 3500) equipped with an electrospray ionization (ESI) source in the positive ion mode. Multiple reaction monitoring (MRM) mode was selected for quantitation through monitoring the precursor-to-parent ion transition at m/z 291.9 → 173.0, m/z 396.9 → 225.1, m/z 388.9 → 217.0, and m/z 146.9 → 91.0 for AW-9a, WES-1, WES-2, and Coumarin (IS), respectively. Linearity was computed using the weighted least-squares linear regression method (1/x2) over a concentration range of 1–1000, 2.5–800, and 5–500 ng/mL for AW-9a, WES-1, and WES-2; respectively. The bioanalytical LC-MS/MS method was fully validated as per U.S. Food and Drug Administration (FDA) guidelines with all respect to linearity, accuracy, precision, carry-over, selectivity, dilution integrity, and stability. The proposed LC-MS/MS method was applied successfully for the determination of all investigated drugs in spiked human plasma with no significant matrix effect, which is a crucial cornerstone in further therapeutic drug monitoring of newly developed therapeutic agents. 相似文献
9.
D. Bhavesh P. Srinivasa P. Parag P. Brijesh R. Shivprakash V. Prashanth Kumar 《Chromatographia》2006,63(5-6):243-248
A simple, rapid, sensitive high performance liquid chromatography method with fluorescent detection was developed and validated
for the determination of bendroflumethiazide in human plasma. Extraction from the plasma was by liquid-liquid extraction using
ethyl acetate. Mosapride citrate was used as the internal standard. The chromatographic separation was performed on reverse
phase LiChrosphere C18 column with mobile phase comprising of acetonitrile and phosphate buffer (38:62 v/v). The assay precision
ranged from 0.9–12.5 and accuracy between 96.8–108.8%, revealing that the method has good reproducibility over the concentration
range of 0.98–100.16 ng mL−1. The validated method has been applied to analyze the bendroflumethiazide concentrations for application in pharmacokinetic,
bioavailability or bioequivalence studies. 相似文献
10.
《Analytical letters》2012,45(17):3245-3255
Abstract In this study, a fast and sensitive liquid chromatography/tandem mass spectrometry method for the determination of captopril in human plasma was developed and validated. The analyte and enalaprilat, used as the internal standard, were extracted from plasma using methanol directly precipitate protein. Analysis was performed on a Lichrospher CN column with water (containing 0.1% formic acid) and methanol (60∶40, v/v) as the mobile phase. Linearity was assessed from 6.25 to 800 ng/ml in plasma. The analytical method proved to be applicable in a pharmacokinetic study of captopril after oral administration of 20 mg captopril tablet to 20 healthy volunteers. 相似文献
11.
A rapid, sensitive, and accurate high-performance liquid-chromatographic–mass spectrometric (HPLC–MS) method, with estazolam as internal standard, has been developed and validated for determination of aripiprazole in human plasma. After liquid–liquid extraction the compound was analyzed by HPLC on a C18 column, with acetonitrile—30 mm ammonium acetate containing 0.1% formic acid, 58:42 (v/v), as mobile phase, coupled with electrospray ionization mass spectrometry (ESI-MS). The protonated analyte was quantified by selected-ion recording (SIR) with a quadrupole mass spectrometer in positive-ion mode. Calibration plots were linear over the concentration range 19.9–1119.6 ng mL−1. Intra-day and inter-day precision (CV%) and accuracy (RE%) for quality-control samples (37.3, 124.4, and 622.0 ng mL−1) ranged between 2.5 and 9.0% and between 1.3 and 3.5%, respectively. Extraction recovery of aripiprazole from plasma was in the range 75.8–84.1%. The method enables rapid, sensitive, precise, and accurate measurement of the concentration of aripiprazole in human plasma. 相似文献
12.
建立了家兔血浆中奥司他韦的高效液相色谱-串联质谱测定方法。以ZORBAX XDB-C18柱为色谱柱,乙腈-0.4%甲酸水溶液为流动相,梯度洗脱;流速300μL.min-1;柱温:20℃。质谱条件为气动辅助电喷雾离子源(ESI),检测方式为正离子多离子反应监测(MRM),以m/z313/166、313/208为定性离子对,m/z313/166为定量离子;生物样品采用固相萃取方法处理。奥司他韦的线性范围为0.05~500μg.L-1,定量下限达0.05μg.L-1,日内、日间相对标准偏差均小于6%,回收率为91%~93%,结果表明该法准确、灵敏、特异,适用于生物样品中奥司他韦的测定。该文还进一步探讨了奥司他韦主要质谱碎片的产生机理。 相似文献
13.
The Validation of an LC-MS Method for the Determination of Risperidone and its Active Metabolite 9-Hydroxyrisperidone in Human Plasma 总被引:1,自引:0,他引:1
Li Zhang Zheng Jiao Zouqing Yao Yan Zhong Mingkang Zhong Yunqiu Yu 《Chromatographia》2005,61(5-6):245-251
A simple, specific and sensitive high performance liquid chromatography-mass spectrometry (LC-MS) method for the determination of risperidone and its active metabolite 9-hydroxyrisperidone in human plasma has been developed and validated. The analytes were prepared through a single-step liquid-liquid extraction (LLE) procedure with the solvent methyl tert-butyl ether and quantitated by MS detection in the positive mode using selected ion monitoring (SIM). Each analytical run was completed within 9 min. Results showed that the LC-MS method enabled to detection of both compounds down to 0.1 ng.mL–1 (S/N > 3) and the linear range was 0.2–24 ng.mL–1, with the correlation coefficients above 0.99. At the concentration of 0.2, 0.5, 10 and 20 ng.mL–1, the inter-day and intra-day RSD were both below 15%. The method has been successfully used to support the routine therapeutic drug monitoring (TDM) and the pharmacokinetics study of risperidone. 相似文献
14.
液相色谱-质谱/质谱法对多种食品基体中三聚氰胺的检测 总被引:2,自引:1,他引:2
采用超声、振荡、液液萃取、离心等方法提取14种复杂食品基体中的三聚氰胺,提取液经阳离子交换固相萃取柱净化后,采用液相色谱-质谱/质谱法测定多种食品基体中的三聚氰胺.涉及的食品基体包括豆类制品、饮料、糕点、含乳饼干、鲜蛋、蛋制品和调味品6类基体14种食品.方法的检出限为0.005 ~0.012 5 mg/kg,回收率为75% ~115%,RSD小于18%;定量下限为0.025 ~0.062 5 mg/kg,回收率为84% ~106%,RSD小于10%.中、高浓度添加回收率为82% ~110%,RSD小于12%.方法灵敏、准确、有效. 相似文献
15.
A method for the simultaneous determination of N-methyl-2-pyrrolidone (NMP) and its metabolites 5-hydroxyl-N-pyrrolidone (5HNMP), N-methylsuccinimide (MSI) and 2-hydroxy-N-methylsuccinimide (2HMSI) in plasma and urine has been developed. Samples were purified by SPE using an ASPEC XL4. Analysis
was performed using LC–MS equipped with an APCI interface. The analysis provided linear responses in the range of 0.125–12 μg
mL−1 for all of the analytes and up to 150 μg mL−1 for 5HNMP and 2HMSI. The within day precision was in the range of 0.9–19.1% for plasma samples and 1.9–10.4% for urine samples
whereas the between day precisions were 4.5–11.9% and 1.2–17.5%, respectively. The method was deemed to be suitable for monitoring
the levels of NMP and its metabolites in the plasma and urine of occupationally exposed persons. 相似文献
16.
A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MS/MS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162.1 for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ng/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199-1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples. 相似文献
17.
高效液相色谱-质谱联用技术测定人血浆中双氢青蒿素的含量 总被引:10,自引:1,他引:9
建立了测定人血浆中的双氢青蒿素的液相色谱 -质谱联用法。色谱条件 :AlltimaC18 柱 (2.1×150mm ,5μm ,流动相 :甲醇 -水 (体积比85∶15) ;流速 :0.2mL/min ;柱温 :25℃ ;进样量 :20μL。质谱条件 :电喷雾离子源 (ESI) ;用于定量分析的离子分别为m/z307(双氢青蒿素) ,m/z275(蒿甲醚 )。样品用液 -液萃取方法处理。双氢青蒿素的线性范围为5~200μg·L -1,定量下限为5μg·L -1,日内、日间精密度 (RSD)均小于10 % ,萃取回收率在71.5 %~83.2 %之间 (n=5) ,分析方法回收率在98.4 %~101.9 %之间 (n=5)。本法操作简便、准确、灵敏度高 ,适用于双氢青蒿素的药代动力学研究 相似文献
18.
J. L. Martínez Vidal A. Garrido Frenich T. López López I. Martínez Salvador L. Hajjaj el Hassani M. Hassan Benajiba 《Chromatographia》2005,61(3-4):127-131
An analytical method for determining residues of twenty pesticides by liquid chromatography (LC) coupled to electrospray ionisation (ESI) tandem mass spectrometry (MS-MS) in eight commodities, cucumber, tomato, pepper, green bean, eggplant, zucchini, melon and watermelon, has been developed and validated. On one hand, calibration curves prepared in solvent were compared with calibration curves prepared in a blank matrix extract of each target matrix. On the other hand, calibration curves and recoveries for each commodity were compared. Cucumber was selected as potential reference matrix for the target vegetables. 相似文献
19.
A rapid and sensitive liquid chromatographic–mass spectrometric (LC–MS) method, with phenoprolamine hydrochloride (DDPH) as
internal standard, has been developed and validated for determination of ranolazine in rat plasma. After liquid–liquid extraction
the compound was analyzed by HPLC on a C18 column, with methanol–10 mM ammonium acetate, 76:24 (v/v), as mobile phase, coupled with electrospray ionization mass spectrometry (ESI–MS). The protonated analyte was quantified
by selected-ion monitoring (SIM) with a quadrupole mass spectrometer in positive-ion mode. Calibration plots were linear over
the concentration range 0.046–12 μg mL−1. Inter and intra-day precision (CV%) and accuracy (RE%) for quality-control samples (0.187, 1.5, and 12 μg mL−1) ranged between 2.96 and 13.38% and between −11.23 and 12.67%, respectively. Extraction recovery of RAN from plasma was in
the range 82.77–86.54%. The method enables rapid, sensitive, precise, and accurate measurement of the concentration of ranolazine
in rat plasma. 相似文献
20.
建立了基于液液萃取/液相色谱-串联质谱法定量分析海水中3种短裸甲藻毒素(BTX-1、BTX-2、BTX-3)。利用液相色谱-串联质谱的高灵敏度,将海水的分析体积减至20 mL;通过响应面优化确定了海水中短裸甲藻毒素的最佳提取条件:加6 g氯化钠,旋涡时间60 s,用5 mL乙酸乙酯提取2次。3种短裸甲藻毒素的线性范围为1~200μg/L,其检出限均为0.02μg/L,定量下限均为0.05μg/L,平均回收率为95.4%~104%,日内相对标准偏差(RSD)为2.2%~5.3%,日间RSD为3.0%~4.5%。方法降低了样品的分析体积,提高了前处理效率,且时效性和适用性强,实现了污染海水中短裸甲藻毒素的高效率痕量分析。 相似文献