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Quantitative determination of glycopyrrolate in human plasma by liquid chromatography-electrospray ionization mass spectrometry: the use of a volatile ion-pairing agent during both liquid-liquid extraction and liquid chromatography

机译:液相色谱-电喷雾电离质谱法定量测定人血浆中的格隆溴铵:在液-液萃取和液相色谱法中使用挥发性离子对试剂

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摘要

The work presented here deals with the development of a quantitative tool for the determination of the quaternary ammonium anticholinergic glycopyrrolate in human plasma samples. Mepenzolate was used as an internal standard. The plasma samples were subjected to a suitable sample clean-up consisting of a simple and relatively fast, two step liquid-liquid ion-pair extraction procedure. The chromatography, using the same volatile ion-pair reagent heptafluorobutyric acid (HFBA), takes only 10 min. Relative standard deviation of retention times was never above 2.26% (n=36). The method was fully validated based on the US FDA Bioanalytical Method Validation Guidance for Industry. As such, a quantitative ESI-LC-MS(/MS) (TOF mass spectrometry) method was optimized for the absolute quantification of glycopyrrolate in human plasma in a concentration range from 0.101 to 101 ng/mL using a quadratic calibration function (R(2)=0.9995), y=-2.21 x 10(-4) (+/-3.93 x 10(-5))xx(2)+5.85 x 10(-2) (+/-5.27 x 10(-3))xx+4.08 x 10(-3) (+/-4.82 x 10(-4)). For the three QC concentrations (QC(1) 0.252, QC(2) 2.52, and QC(3) 25.2ng/mL) and the LLOQ (0.101 ng/mL), total precision was under 20% (18.0% (n=6) at the LLOQ) and maximum accuracy was 112% (88.9% for the LLOQ, n=6). Absolute matrix effect (maximum 133%+/-9.59, n=3), absolute recovery (better than 41.8%+/-2.22, n=3), relative (inter-subject) matrix effect (maximum 10.9%+/-1.45, n=4) and process efficiency (better than 45.2%+/-5.74, n=3) too were assessed at the 3 QC concentrations.
机译:本文介绍的工作涉及定量工具的开发,该工具可用于测定人血浆样品中的抗胆碱能格隆溴铵季铵盐。甲苯甲酸酯用作内标。对血浆样品进行适当的样品净化,包括简单且相对快速的两步液-液离子对萃取程序。使用相同的挥发性离子对试剂七氟丁酸(HFBA)进行色谱分析仅需10分钟。保留时间的相对标准偏差从未超过2.26%(n = 36)。该方法已根据美国FDA工业用生物分析方法验证指南进行了充分验证。因此,优化了定量ESI-LC-MS(/ MS)(TOF质谱)方法,使用二次校准函数对R(0.12)浓度范围从0.101至101 ng / mL的人血浆中的格隆溴铵进行绝对定量(R( 2)= 0.9995),y = -2.21 x 10(-4)(+/- 3.93 x 10(-5))xx(2)+5.85 x 10(-2)(+/- 5.27 x 10(-3) ))xx + 4.08 x 10(-3)(+/- 4.82 x 10(-4))。对于三个QC浓度(QC(1)0.252,QC(2)2.52和QC(3)25.2ng / mL)和LLOQ(0.101 ng / mL),总精度低于20%(18.0%(n = 6)在LLOQ),最大精度为112%(LLOQ为88.9%,n = 6)。绝对基质效应(最大133%+ /-9.59,n = 3),绝对恢复(优于41.8%+ /-2.22,n = 3),相对(受试者间)基质效应(最大10.9%+ /-1.45) ,n = 4)和过程效率(优于45.2%+ /-5.74,n = 3)也在3个QC浓度下进行了评估。

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