LC-MS/MS法测定酸枣仁中赭曲霉毒素A

Determination of ochratoxin A in ziziphi spinosae seme by LC-MS/MS

目的建立酸枣仁中赭曲霉毒素A的LC-MS/MS测定方法,着重于方法的提取与净化、质谱参数的分析等过程。方法以酸枣仁为研究基质,采用改良Qu ECh ERS法,均质样品经水浸泡后,加入10%甲酸-乙腈溶液进行提取,同时加入莠去津作为内标;乙腈溶液经分散固相萃取技术净化后,用高效液相色谱-串联质谱法进行分析测定。结果赭曲霉毒素A在0.05 ng/ml^5 ng/ml时进样量与峰面积呈良好的线性关系,加样回收率为72.11%~85.00%。方法的重复性及稳定性均良好;检出限为0.1μg/kg。改良Qu ECh ERS法既省时又经济有效。结论本法简便快速、灵敏度高、结果准确,可用于酸枣仁中赭曲霉毒素A的测定分析。

Objective To develop a method for determining ochratoxin A in ziziphi spinosae seme,and especially focused on the optimization of extraction,clean- up,MS / MS parameters of analytes. Methods Homogenized samples of ziziphi spinosae seme were extracted by Qu ECh ERS,with the selected internal standard（ atrazine） spiking. The extract was purified by d- SPE. Ochratoxin A was analyzed by LC- MS / MS. Results The calibration curve was linear within the range of 0. 05 ng / ml- 5. 00 ng / ml.The recoveries were among 72. 11%- 85. 00%. Repeatability and stability were good. Limit of detection was 0. 1 μg / kg. The Qu ECh ERS approach was with less time and cost- effective. Conclusion The method is simple,sensitive and accurate and it is suitable for the determination of ochratoxin A in ziziphi spinosae ssemen.