气相色谱-电子捕获法测定人血中舍曲林及其代谢产物去甲舍曲林的浓度

Determination of sertraline and desmethylsertraline in human plasma by gas chromatography with electron capture detector

目的 :建立一种测定人血浆中舍曲林及其代谢产物去甲舍曲林浓度的方法。方法 :在碱性条件下用乙醚 正己烷 (80∶2 0 ,V/V)一次萃取 ,并以 10 %的三氟醋酐在 5 0℃下进行衍生化处理。采用 5 %苯基石英毛细管柱 (30m× 0 .2 5mm ,0 .2 5 μm) ,柱温 2 37℃。高纯度N2 为载气 ,流速 0 .75mL·min-1,分流比 2 5∶1,柱前压 115kPa。进样口温度 2 6 0℃ ,63 Ni电子捕获检测器 ,检测器温度 30 0℃。结果 :舍曲林和去甲舍曲林的线性范围均为 1.0～ 10 0 μg·L-1,最低检测浓度 0 .5 μg·L-1,相对回收率分别为96 .8%～ 10 8.2 %和 94 .5 %～ 10 6 .7% ,日内和日间RSD <8.5 %。结论 :本法简便、准确、灵敏 ,重现性好 。

AIM: To develop a gas chromatography (GC) method with electron-capture detection for the simultaneous determination of sertraline and its primary metabolite desmethylsertraline in human plasma. METHODS: After one-step extraction with diethyl ether and hexane (80∶20,V/V) at pH>10.5, the extracted samples were derivatized with trifluoroacetic anhydride (TAFF) at 50℃. Runs were performed on a 5% phenylmethyl silicone capillary column (30 m×0.25 mm, 0.25 μm). The column pressure was 115 kPa, the flow rate was 0.75 mL·min -1, and the split ratio was 25∶1. The temperature of injector was 260℃, and the temperature of 63Ni electron capture detector was 300℃. RESULTS: The response was linear over the range of 1.0 μg·L -1 to 100 μg·L -1 for sertraline and desmethylsertraline, and the lower limits of assay were 0.5 μg·L -1. The relative recovery (94%-108%) had good precision with relative standard deviation of less than 8.5%. CONCLUSION: This method is simple and reproducible, and the results are reliable and accurate.