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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 a method for the determination of niclosine content in human blood by GC-MS. Methods: Samples were adjusted to basicity with borax buffer solution at pH 8.98, extracted with ether, suspended and centrifuged. The organic layer was air-dried with nitrogen and the residue methanol was centrifuged. The supernatant was analyzed by GC / MS. A, qualitative characteristic ions 108, 322, quantitative characteristic ions 108. Results: The linear range was 0.5-400μg / ml (r = 0.9994). The detection limit was 0.03μg / ml, the precision was 5.8% and the stability was 7.8%. The recovery was 63.8% ~ 66.9%, matrix effect was 128.0%. Conclusion: The method is simple, accurate and can be used as a method for determination of niclosine content in human blood.