摘要
目的 建立测定人全血中百草枯浓度的高效液相串联质谱电喷雾检测法 (LC/MS/MS) 。 方法 以 Waters 公司 C18 反相柱（ Symmetry C18 column ， 4.6 mm × 50 mm ， 5 μ m ）为色谱柱，流动相为乙腈 - 水（含 0.3% 三氟醋酸） =5 ∶ 95 ，流速为 0.3 mL·min-1 ，以乙腈沉淀蛋白法提取百草枯。样品经电喷雾离子源正离子化后，通过三重四级杆串联质谱仪，采用选择反应监测（ SRM ）对百草枯（ <> m/z 185.2 → 169.1 ）进行测定，并将此法应用于临床监测患者血中百草枯浓度。 结果 百草枯的高（ 5 mg·L-1 ）、中（ 1.25 mg·L-1 ）、低（ 0.08 mg·L-1 ） 3 个质量浓度的平均回收率分别为 71.80% ， 70.77% 和 77.84% ，日内（ <> n =5 ）、日间（ <> n =3 ） RSD 均小于 15% ；分析方法的最低定量限为 0.04 mg·L-1 。线性范围为： 0.04 ～ 10 mg·L-1, 回归方程为 <> y =10 200<>x+309 ， <> r =0.998 8 （ <> n =8 ）。 结论 该方法灵敏、准确、简单、快速，可用于临床检测患者血中百草枯浓度。
Abstract
OBJECTIVE To develop a LC/MS/MS method for the determination of paraquat assay in whole blood. METHODS The sample were pretreated with the precipitation of protein with acetonitrile and separated on a Waters Symmetry C18 column (4.6 mm×50 mm，5 μm ) with the mobile phase consisting of acetonitrile: water with 0.3% trifluoroacetic acid (95∶5). The flow rate was 0.3 mL·min-1. A API3200 triple quadmass spectrometer system equipped with an electrospray ionization source was used as the detector and operated in the positive ion mode. Selected reaction monitoring (SRM) was used with the precursor to product ion combinations of m/z 185.2→169.1. The method was used to measure paraquat in whole blood of patient. RESULTS ■The average recoveries of paraquat were 71.80%, 70.77% and 77.84% at three concentration levels of 5, 1.25, 0.08 mg·L-1, respectively. The relative standard deviations from intra-day (n=5) and inter-day (n=3) precision were less than 15%. The calibration curves for paraquat had good linearity（r=0.998 8，n=8）over the range of 0.04-10 mg·L-1. The limits of quantification for paraquat was 0.04 mg·L-1. CONCLUSION The method provides a sensitive, accurate, precise and reliable analytical procedure for clinical monitoring of paraquat blood sample.
关键词
高效液相色谱 - 串联质谱法 /
百草枯 /
全血浓度
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Key words
LC/MS/MS /
paraquat /
whole blood concentration
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邱葵;吴华;张征;徐佳佳;杨梅;孔繁翠;王鹤尧 .
LC-MS/MS 测定患者全血中百草枯的浓度[J]. 中国药学杂志, 2009, 44(16): 1259-1261
QIU Kui;WU Hu;ZHNG Zheng;XU Ji-ji;YNG Mei;KONG Fn-cui;WNG He-yo .
Determination of Paraquat in Whole Blood by LC/MS/MS Assay[J]. Chinese Pharmaceutical Journal, 2009, 44(16): 1259-1261
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参考文献
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（收稿日期： 2009-04-28 ）
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