水中2种微囊藻毒素及3种农药的固相萃取-超高效液相色谱-串联质谱测定法

Simultaneous determination of two microcystins and five pesticides in water by solid-phase extraction and ultra high performance chromatography-tandem mass spectrometry

目的建立水中2种微囊藻毒素(MC-LR、MC-RR)、呋喃丹、甲萘威和莠去津的固相萃取-超高效液相色谱-串联质谱(UPLC-MS-MS)测定法。方法采用HLB固相萃取柱对水中5种有害物质进行富集净化,利用ZORBAX Eclipse XDB C_(18)色谱柱分离待测物,以0.2%甲酸水-乙腈为流动相进行梯度洗脱,以正离子喷雾模式电离,以MRM方式进行质谱分析。结果在0.1～25μg/L的线性范围内,所得5种目标化合物的回归方程均呈较好的线性关系(r>0.999)。该方法的检出限为0.000 3～0.015 0μg/L,定量下限为0.001～0.040μg/L;平均回收率在76.5%～102.0%之间,RSD<5%。结论该方法简便、灵敏、准确,适用于水中5种物质的日常批量检测。

Objective To establish the method for determination of two kinds of microcystins,carbofuran,carbaryl and atrazine in water by solid-phase extraction and ultra high performance chromatography-tandem mass spectrometry (UPLC-MS-MS). Methods The five toxicants in water were concentrated and purified by HLB SPE column and then separated on ZORBAX Eclipse XDB C18 chromatographic column with mobile phase of 0.2%formic acid water and acetonitrile by gradient elution. Multiple reaction monitoring (MRM)mode was used for mass spectrometry determination.Results In the linear range of 1.0- 25.0μg/L,the regression equations of the five target compounds showed a good linear relationship (r>0.999).The limits of detection for five compounds were 0.0003-0.015μg/L,the average recovery rates ranged from 76.5% to 102.0%,and RSD< 5%.Conclusion The method is simple,sensitive,accurate and suitable for daily batch testing of five kinds of harmful substances in water.