摘要
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,3.5μm)分离,分别在电喷雾正、负离子模式下以多反应监测(MRM)方式检测。正离子模式下的流动相为水-乙腈,负离子模式下的流动相为0.1%氨水-乙腈。结果表明,30种药物在相应的质量浓度范围内线性良好,相关系数均大于0.99,在3个加标水平下的平均回收率为63%～118%,相对标准偏差(RSD)为3.8%～18.2%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.03～1.6μg/kg及0.10～5.0μg/kg。市售多种鲜活鱼类的测定结果表明,该方法简便快速、灵敏可靠、经济有效,适用于鱼肉中激素类及氯霉素类药物多残留的同时快速测定。
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 - 5.0μg/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.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第12期1329-1337,共9页
Journal of Instrumental Analysis
基金
广东省科技计划重点专项"农产品检测监控与追溯技术研究与示范"资助项目(2009A020101004)
关键词
QUECHERS
液相色谱-串联质谱
雌激素
雄激素
孕激素
糖皮质激素
氯霉素
鱼肉
QuEChERS
liquid chromatography - tandem mass spectrometry （ LC - MS/MS）
estrogens
androgens
progesterones
glucocorticoids
chloramphenicols
fish
