亲水作用液相色谱-串联质谱测定水产品中的消毒剂残留

首次建立了水产品中消毒剂二氯异氰尿酸和三氯异氰尿酸总残留量以及三氯生残留量的液相色谱-串联质谱(LC-MS/MS)同时测定方法。水产样品用乙腈-5%氨水(体积比30∶70)提取,HyperSep RetainAX SPE固相萃取小柱净化,采用亲水作用色谱柱SeQuant ZIC-HILIC分离,以(0.1%甲酸+10 mmol/L乙酸铵)水溶液-乙腈体系为流动相进行梯度洗脱,在电喷雾负离子模式下以多反应监测(MRM)方式检测。结果表明,在0.042～2.4 mg/L质量浓度范围内线性良好,相关系数大于0.99,在3个不同加标水平下,平均回收率为68%～96%,相对标准偏差(RSD)为5.9%～10.9%,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.015、0.05 mg/kg。实际样品测定表明,该方法适用于各种水产品中三氯生、二氯异氰尿酸和三氯异氰尿酸消毒剂残留量的测定。

Determination of Aquaculture Disinfectants Residues in Aquatic Products by Hydrophilic Interaction Liquid Chromatography-Tandem Mass Spectrometry

A new method for the determination of 3 aquaculture disinfectants in aquatic products using hydrophilic interaction liquid chromatography-tandem mass spectrometry(LC-MS/MS) was established.The homogenized sample was extracted with acetonitrile-5% ammonia hydroxide(30 ∶ 70,by volume).Separation of analytes was performed using a SeQuant ZIC-HILIC hydrophilic interaction column by gradient elution after solid-phase extraction(SPE) purification.The qualitative and quantitative analyses of 3 aquaculture disinfectants were operated by electrospray ionization mass spectrometry under the negative mode using multiple reaction monitoring(MRM).Acetonitrile and water with 0.1% formic acid and 10 mmol/L ammonium acetate were used as the mobile phase.The calibration curves were linear in the range of 0.042-2.4 mg/L with correlation coefficients more than 0.99.The average recoveries at three spiked concentration levels varied from 68% to 96% with relative standard deviations(RSDs) of 5.9%-10.9%.The limit of detection(LOD,S/N≥3) and limit of quantitation(LOQ,S/N≥10) were 0.015 mg/kg and 0.05 mg/kg,respectively.The real sample tests showed that the method was suitable for the determination of aquaculture disinfectants in aquatic products.