水中灭草松、莠去津、2, 4-滴、呋喃丹和微囊藻毒素UPLC-MS-MS快速测定方法

单晓梅; 谢继安; 沈登辉; 刘柏林; 陆蓓蓓; 王冰霜

水中灭草松、莠去津、2, 4-滴、呋喃丹和微囊藻毒素UPLC-MS-MS快速测定方法

Rapid Determination of Bentazone, Atrazine, 2, 4-D, Cavbofuran and Microcystins in Water by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

摘要

摘要:
目的建立同时快速测定水中灭草松、莠去津、2, 4-滴、呋喃丹和微囊藻毒素化合物超高效液相色谱-串联质谱方法。
方法直接或离心后取上清液进样, 利用Acquity BEH C₁₈色谱柱分离待测物, 串联质谱仪检测, 以乙腈和0.1%甲酸水溶液为流动相梯度洗脱, 流速0.3 mL/min, 外标法定量。
结果灭草松、2, 4-滴、莠去津、呋喃丹、微囊藻毒素-RR、微囊藻毒素-LR 6种化合物线性浓度范围分别为1.0~50.0、1.0~50.0、0.5~25.0、1.0~50.0、0.2~10.0和0.2~10.0 μg/L, 其线性相关系数均大于0.999, 6种化合物的方法检出限为0.01~0.1 μg/L, 回收率为98.0%~102.1%, 相对标准偏差为1.73%~3.06%。
结论该法简便、准确, 适用于生活饮用水中多种农药和微囊藻毒素的快速分析。

Abstract:
Objectives To establish an analytical method for the rapid determination of bentazone, atrazine, 2, 4-Dichlorophenyloxy acetic acid (2, 4-D), carbofuran and two microcystins in water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS).
Methods Water samples were injected directly or injected after centrifugation. The determinants were separated by acquity BEH C₁₈ column with acetonitrile and 0.1% formic acid water as mobile phase and gradient elution at a flow rate of 0.3 mL/min, detected by UPLC/MS/MS and quantified by external standards.
Results The linear ranges for bentazone, 2, 4-D, atrazine, carbofuran, microcystins-RR and microcystins-LR were 1.0~50.0, 1.0~50.0, 0.5~25.0, 1.0~50.0, 0.2~10.0, 0.2~10.0 μg/L, respectively. The linear correlation coefficient in proper range was higher than 0.999. The minimum detectable concentration was 0.01~0.1 μg/L; the recovery was 98.0%~102.1%; and the relative standard deviation (RSD) was 1.73%~3.06%. These pesticides were not detected in drinking water of some urban areas in Anhui province.
Conclusions This method is simple and accurate, and suitable for the determination of these compounds in water.

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