QuEChERS/液相色谱-串联质谱法同时测定鱼肉中30种激素类及氯霉素类药物残留

建立了鱼肉中8种雌激素、5种雄激素、6种孕激素、8种糖皮质激素及3种氯霉素类药物多残留的QuEChERS/液相色谱-串联质谱(LC - MS/MS)同时测定方法.均质样品用水分散后加乙腈提取,经分散固相萃取净化后,采用ZORBAX Extend-C18色谱柱(100 mm ×2.1 mm,3.5 μm)分离,分别在电喷...

Simultaneous Determination of 30 Hormones and Chloramphenicols Residues in Fish Using QuEChERS Sample Preparation and Liquid Chromatography-Tandem Mass Spectrometry

A multi-residue method was developed for the simultaneous determination of 8 estrogens,5 androgens,6 progesterones,8 glucocorticoids and 3 chloramphenicols in fish using QuEChERS sample preparation and liquid chromatography-tandem mass spectrometry(LC-MS/MS).The homogenized sample was dispersed by water,then the analytes were extracted with acetonitrile.The separation were performed on a ZORBAX Extend-C18 column(100 mm×2.1 mm,3.5 μm) by gradient elution after dispersive-solid-phase extraction(d-SPE) purification.The qualitative and quantitative analysis of 30 analytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring(MRM).Acetonitrile and water were used as the mobile phase in the positive mode.Acetonitrile and 0.1% ammonia hydroxide were used as the mobile phase in the negative mode.The correlation coefficients of calibration curves were over 0.99 in the corresponding concentration range.The average recoveries of the 30 analytes at three spiked concentration levels varied from 63% to 118% with relative standard deviations(RSDs) of 3.8%-18.2%.The limits of detection(LOD,S/N≥3) and quantitation(LOQ,S/N≥10) were 0.03-1.6 μg/kg and 0.1-5.0 μg/kg,respectively.The real sample tests showed that the proposed method was simple,rapid,sensitive,reliable and cost-effective,and was suitable for the simultaneous determination of hormones and chloramphenicols in fish samples.