高压液相色谱-串联质谱法检测食物中毒样品中的乌头碱

Determination of aconitine in food poisoning samples by high pressure liquid chromatography-tandem mass spectrometry

目的建立引起食物中毒的芝麻糊中乌头碱的高压液相色谱-串联质谱(HPLC-MS/MS)测定方法。方法样品经0.1%甲酸-2mmol/L甲酸铵缓冲溶液振荡提取后,离心、过滤,以等体积比的甲醇和甲酸-甲酸铵缓冲溶液为流动相,经C18色谱柱分离后以多反应监测质谱测定。结果方法的线性范围为1～1000μg/L,线性相关系数为0.999,最低定量浓度(LOQ)为10μg/kg,在50～5000μg/kg添加水平下平均回收率为82%～94%,相对标准偏差(RSD)为4.9%～7.4%。结论该方法能够满足食物中毒样品中乌头碱的检测。

Objective To establish an analytical method for determination of aconitine in poisoning se-same paste samples by high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Samples were extracted by formic acid (0.1%)-ammonium formate (2 mmol/L) buffer. The extract was centrifuged and filtered by 0.45μm nylon membrane filters before being analyzed with HPLC-MS/MS. A Waters Acquity BEH C18 column (2.1 mm×50 mm, 1.7μm) was adopted with the mobile phase of methanol and formic acid (0.1%)-ammonium formate (2 mmol/L) buffer (1:1, v/v). Aconitine was detected by high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) under multiple reactions monitoring (MRM) mode. Results The method showed a good linearity in the range of 1~1000μg/L with correlation coefficients of 0.999, and the LOQ was 10 μg/kg. The average recoveries were 82%~94% at the spiked level of 50~5000μg/kg with the relative standard deviation (RSD) of 4.9%~7.4%. Conclusion This method can meet require-ments of fast and accurate determination of aconitine in food poisoning samples.