GC/MS法测定人血中钩吻碱甲

Determination of gelsemine in human blood by GC /MS

目的：建立GC-MS法测定人血中钩吻碱甲含量的方法。方法：样品用pH 8.98的硼砂缓冲溶液调至碱性,经乙醚提取、混悬、离心,取有机层氮气吹干,残渣甲醇定容,离心,上清液GC/MS分析,测定钩吻碱甲,定性特征离子108、322,定量特征离子108。结果：钩吻碱甲在0.5-400μg/ml范围内与峰面积呈现良好的线性关系（r=0.9994）,检测限为0.03μg/ml,方法精密度5.8%,稳定性7.8%,回收率为63.8%-66.9%,基质效应为128.0%。结论：方法操作简便,结果准确,可作为测定人血中钩吻碱甲含量的方法。

Objective：To establish the method of gas chromatography with mass spectrometry for determination of gelsemine in blood. Methods：pH 8.98 borax buffer solution adjusted to alkaline samples, extracted with ether, suspension, centrifugation, the organic layer is dried with nitrogen, residue by methanol volume, after centrifugation supernatant sample analysis, determination of gelsemine, qualitative characteristic ions, 108,322, 108 quantitative characteristic ion. Results：Gelsemine in 0.5 - 400 μg/ml scope with the peak area showed a good linear relationship （r =0. 9994）, the detection limit is 0.03 μg/ml, precision 5.8%, method 7.8%, the recovery rate was 63.8% - 66.9%, the matrix effect was 128%. Conclusion：The method was simple, sensitive, accurate and repeatable. It can be used for determination of gelsemine in human blood.