建立了QuEChERS一种分散型固相萃取（QuEChERS）与高效液相色谱-串联质谱（HPLC-MS/MS）联用测定水产品中二甲戊灵的方法。样品采用含0.1%（体积分数）甲酸的乙酸乙酯提取，提取液经0.6 g聚苯乙烯-二乙烯基苯和0.2 g乙二胺-N-丙基硅烷分散固相萃取净化，40 ℃下氮吹浓缩近干，加入乙腈1.0 mL复溶，经0.22 μm滤膜过滤，高效液相色谱-串联质谱测定。目标化合物采用Kinetex C18色谱柱（100 mm×2.1 mm，2.6 μm）分离，采用乙腈和0.1%（体积分数）甲酸水溶液进行梯度洗脱，在电喷雾离子源（ESI）、选择反应监测（SRM）模式下进行测定，基质匹配内标法定性定量。结果表明，目标物在2~100 μg/L范围内线性关系良好，相关系数为0.999 5，检出限（LOD）和定量限（LOQ）分别为0.5 μg/kg和1.0 μg/kg。以鲤鱼、克氏原螯虾和中华鳖为样品基质，在3个不同的添加水平下，二甲戊灵的平均回收率为78.9%~110.6%，RSD为3.8%~6.8%。该方法具有快速、准确度与灵敏度高的优点，满足稻田水产品中二甲戊灵的残留检测需求。

A method based on Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) dispersive solid-phase extraction coupled with high performance liquid chromatography tandem mass spectrometry was developed for the determination of pendimethalin in aquatic products. The samples were extracted with ethyl acetate containing 0.1% (V/V) formic acid, and the extracts were purified by dispersive solid-phase extraction with 0.6 g polystyrene-divinylbenzene (PS-DVB) and 0.2 g primary secondary amine (PSA) sorbents. The purified extracts were collected and concentrated at 40 ℃ to almost dry under nitrogen gas. The resulting extracts were re-dissolved in 1.0 mL of acetonitrile, filtered through microfiltration membrane (0.22 μm), and analyzed by high performance liquid chromatography-tandem mass spectrometry. The target compounds were separated on a Kinetex C18 column (100 mm×2.1 mm, 2.6 μm), and gradient elution was performed with acetonitrile and 0.1% (V/V) aqueous formic acid solution. Electrospray ion source (ESI) and selective reaction monitoring (SRM) were used for analysis, and the matrix-matched internal standard method was used for qualitative and quantitative determinations. The results showed that good linear relationship was in the range of 2~100 μg/L, with the correlation coefficient being 0.999 5. The limits of detection (LOD) and quantitation (LOQ) were 0.5 μg/kg and 1.0 μg/kg, respectively. The average recoveries of pendimethalin at three different spiking levels in a sample matrix carp, procambarus clarkiir or pelodiscus sinensis ranged from 78.9% to 110.6%, with RSDs ranging from 3.8% to 6.8% under. This method has the advantages of high speed, accuracy and sensitivity, and can meet the requirements for detecting pendimethalin residue in aquatic products from rice fields.

湖南省科技重大专项资金资助项目（2017NK1030）