高效液相色谱-电喷雾串联三重四级杆质谱法测定水中微囊藻毒素

Determination of Microcystin in Water by HPLC-MS/MS

目的研究利用固相提取净化、高效液相色谱-电喷雾串联三重四级杆质谱检测分析水中微囊藻毒素MC-LR和MC-RR。方法水样品经玻璃纤维滤纸过滤后,经C18固相提取柱富集净化,氮吹后定容。流动相中添加0.1%甲酸,采用梯度洗脱模式,经C18反相色谱柱分离,以电喷雾串联三重四级杆质谱定性、定量测定。结果线性定量范围0.1-5.0μg/kg,检测低限为MC-LR 0.01μg/kg,MC-RR 0.02μg/kg。结论此方法操作简便、定性定量能力较强,可作为检测水质量和评估食品安全风险的可靠方法。

Objective To detect microcystin-LR and microcystin-RR in water by HPLC-MS/MS. Methods The samples were filtered through the glass fiber filter, and purified by C 18 solid phase extraction column, then concentrated through N2 blowing. With adding 0.1%（v/v） formic acid to the mobile phase, chromatographic separation was performed on a C18 reverse column by gradient elution mode, and the analyte was determined by HPLC-MS/MS. Results The linear determination range was 0.1-5.0 μg/kg, and the detection limit was 0.01 μg/kg for microcystin- LR, 0.02 μg/kg for microcystin-RR. Conclusion The method can be easy to operate, and suitable for water sample detection and food safety risk assessment.