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目的建立血液中45种常见有毒生物碱的液相色谱-串联质谱(LC-MS/MS)筛选分析方法。方法目标物的鉴别主要依据化合物的保留时间及其两对离子比对。通过液液提取,运用LC-MS/MS多反应监测,以SKF525A为内标,1 m L血液在p H=9.2条件下用乙醚提取,目标化合物在LC-MS/MS正离子模式下得以分析。结果目标生物碱线性良好(r>0.995 1),日内及日间精密度均小于14.77%。血液中检出限范围为0.05~25 ng/m L。结论该方法运行时间为12 min,对常见有毒生物碱的检出具有良好的选择性及灵敏度,因此被成功运用于多例疑似生物碱急性中毒案例的分析中。
Objective To establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) screening assay for 45 common toxic alkaloids in blood. Methods The identification of the target is based primarily on the retention time of the compound and on its two pairs of ions. LC-MS / MS multiple reaction monitoring with SKF525A as an internal standard and 1 mL of blood were extracted with ether at pH = 9.2 and the target compound was analyzed by LC-MS / MS positive ion mode . Results The target alkaloids had a good linearity (r> 0.995 1) with a precision of less than 14.77% within and between days. The detection limit in blood ranged from 0.05 to 25 ng / m L. Conclusion The method runs for 12 min and has good selectivity and sensitivity for the detection of common toxic alkaloids. Therefore, the method has been successfully applied in the analysis of many cases of acute alkaloid poisoning.