| HPLC-MS/MS法测定血浆中华法林对映异构体浓度 |
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| 引用本文： | 沈艳聪,向 瑾,梁茂植等. HPLC-MS/MS法测定血浆中华法林对映异构体浓度[J]. 四川大学学报(医学版), 2016, 47(1): 106-110 |
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| 作者姓名： | 沈艳聪 向 瑾 梁茂植等 |
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| 作者单位： | 1.四川大学华西医院 临床药理研究室 |
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| 摘 要： | 目的 建立高效液相色谱串联质谱法（HPLC-MS/MS）测定人血浆中华法林对映异构体的浓度。方法 以乙酸乙酯为萃取剂，采用MS Chiral? MS-OD(50×2.1 mm, 3 μm)为手性柱，流动相为甲醇∶水∶甲酸=85∶15∶0.05，流速为0.18 mL/min。采用负离子模式，电喷雾离子源（ESI），以萘普生为内标定量，华法林和内标的检测离子对质荷比分别为（m/z）307.2→160.9和（m/z）228.9→185.1。结果 R-华法林批内精密度，其相对标准偏差(RSD)为3.2%~5.8%,批间RSD为2.5%~5.1%；方法回收率(96.1±5.6)%~(105.4±4.7)%，提取回收率80.7%~84.4%，内标基质效应校准后的基质效应RSD<10%；S-华法林批内精密度RSD为3.7%~5.2%,批间RSD为3.2%~4.8%；方法回收率(98.3±5.1)%~(103.7±3.8)%，提取回收率81.3%~84.6%，内标基质效应校准后的基质效应RSD<10%。最低定量限均为0.1 μg/mL。结论 本文建立的方法准确、灵敏、可靠，可用于人血浆中华法林对映体的拆分和血药浓度的测定。
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| 关 键 词： | 高效液相色谱串联质谱法 华法林对映异构体 血药浓度 |
Determination of Warfarin Enantiomers in Human Plasma with HPLC-MS/MS |
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| SHEN Yan-cong,XIang Jin,LIang Mao-zhi,et al. Determination of Warfarin Enantiomers in Human Plasma with HPLC-MS/MS[J]. Journal of Sichuan University. Medical science edition, 2016, 47(1): 106-110 |
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| Authors: | SHEN Yan-cong XIang Jin LIang Mao-zhi et al |
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| Abstract: | Objective To establish a high performance liquid chromatography-mass spectrometry/mass spectrometry (HPLC-MS/MS) method for determination of warfarin enantiomers in human plasma. Methods Warfarin enantiomers were extracted with ethyl acetate. The HPLC-MS/MS method used naproxen as internal standard, with methanol∶water∶formic acid=85∶15∶0.05 as mobile phase, at a flow rate of 0.18 mL/min. R-warfain, S-warfarin and internal standard (IS) were separated on column MS Chiral?MS-OD (50×2.1 mm, 3 μm). Warfarin enantiomers were protonated with electroapry ionization (ESI) in negative electron ionization mode. The ion pairs being detected were (m/z) 307.2→160.9 (R-warfain and S-warafrin) and (m/z) 228.9→185.1 (IS). Results The within-run precision relative standard deviations (RSD) and between-run precision RSDof R-warfarin were 3.2%-5.8% and 2.5%-5.1%, respectively. The method recoveries and extraction recoveries of R-warfarin were (96.1±5.6)%-(105.4±4.7)% and 80.7%-84.4%, respectively. The matrix effect RSD was less than 10%. The within-run precision RSD and between-run precision RSDof S-warfarin were 3.7%-5.2% and 3.2%-4.8%, respectively. The method recoveries and extraction recoveries of S-warfarin were (98.3±5.1)%-(103.7±3.8)% and 81.3%-84.6%, respectively. The limit of quantification was 0.1 μg/mL for both analytes. Conclusion This new method is fully validated with satisfactory accuracy and adequate reproducibility. Therefore, it can be applied for separating and detecting plasma warfarin enantiomers. |
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| Keywords: | HPLC-MS/MS Warfarin enantiomers Plasma concentration |
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