人血浆中茴三硫代谢产物浓度的LC-MS/MS法测定

Determination of the Metabolite of Anetholtrithion in Human Plasma by LC-MS/MS

建立了LC-MS/MS法测定人血浆中茴三硫代谢产物对羟基茴三硫的浓度。采用Thermo Hypersil Gold色谱柱,流动相为乙腈-水(含0.5‰甲酸)(88∶12),氯雷他定为内标。采用ESI+电离源模式,选择正离子监测质荷比(m/z)为186.3→242.6(对羟基茴三硫)和337.3→383.4(氯雷他定)。样品用乙酸乙酯-异丙醇(95∶5)液液萃取,对羟基茴三硫在15.6～1000μg/L浓度范围内线性良好,批内和批间RSD小于7.10%,方法回收率为98.9%～110.1%。

A LC-MS/MS method was established for the determination of the concentration ofp-hydroxyan etholtrithion, the metabolite of anetholtrithion, in human plasma. A Thermo Hypersil Gold column was used, with the mobile phase of acetonitrile-water （containing 0.5‰ formic acid） （88 ： 12）, the flow rate was 0.25ml/min. Loratadine was used as the internal standard. The analytes were ionized in the ESI ion source of the mass spectrometer and detected in the selected reaction monitoring （SRM） mode （m/z 186.3→242.6 for p-hydroxyl-anetholtrithion and 337.3→383.4 for loratadine）. The plasma samples were extracted by ethylacetate- isopropyl alcohol （95 ： 5）. The calibration curve of p-hydroxyanetholtrithion was linear in the concentration range of 15.6 - 1000μg/L. The average recovery was 98.9% - 110.1%, and RSDs of within- and between-batch were less than 7.10 %.