分析测试学报2017，Vol.36Issue(8)：955-962,8.DOI:10.3969/j.issn.1004-4957.2017.08.002
改良的QuEChERS与HPLC-HESI/MS/MS同时测定中华鳖组织中氯硝柳胺和酰胺醇类药物及其代谢物的残留量
Determination of Niclosamide and Amphenicols Residues in Chinese Soft-shelled Turtle(Trionyx sinensis) Tissues by Modified QuEChERS Combined with HPLC-HESI/MS/MS
摘要
Abstract
A modified QuEChERS sample preparation combined with high performance liquid chromatography-heated electrospray ionization-tandem mass spectrometric (HPLC-HESI/MS/MS) method was established for the simultaneous determination of niclosamide (NIC),chloramphenicol (CAP),thiamphenicol (TAP),florfenicol (FF) and florfenicol amine (FFA) in plasma,muscle,skirt,liver and kidney of Chinese soft-shelled turtle (Trionyx sinensis).The sample was extracted and purified using a modified QuEChERS method,and ammoniate acetonitrile and octadecyl silane (C18) were chosen as extractant and purification,respectively.The mobile phase comprised of methanol and water,and the flow rate was set at 0.3 mL/min.The sample prepared was separated on a Waters Symmetry（R） C18 (2.1 mm × 100 mm,3.5 μm) column,and determined in the positive and negative ion multiple reaction monitoring mode through polarity switching between time segments.CAP,TAP,FF and FFA were quantified by internal standard calibration curve method,and NIC was used the external standard matrix-matched standard curve method.Good linearities were observed in the range of 0.3-100 μg/L for five analytes,with correlation coefficients not more than 0.998 7.The average recoveries of 5 analytes at the spiked level of 1-20 μg/kg in plasma,muscle,skirt,liver and kidney of Chinese soft-shelled turtle(Trionyx sinensis) ranged from 77.9％ to 105.3％ with relative standard deviations(RSD) of 2.7％-10.5％.The detection limits(LOD) for NIC,CAP,TAP,FF and FFA in Chinese soft-shelled turtle tissues were 0.5,0.1,0.5,0.5,0.5 μg/kg,and the quantitation limits(LOQ) were 1.0,0.3,1.O,1.0,1.0 μg/kg,respectively.The method is simple,accurate,highly sensitive,and is suitable for the simultaneous determination of NIC,CAP,TAP,FF and FFA residues in Chinese soft-shelled turtle tissues.关键词
中华鳖/氯硝柳胺/酰胺醇类/改良的QuEChERS/高效液相色谱-加热电喷雾电离源串联质谱Key words
Chinese soft-shelled turtle/niclosamide/amphenicols/modified QuEChERS/high performance liquid chromatography-heated electrospray ionization-tandem mass spectrometry (HPLC-HESI/MS/MS)分类
化学化工引用本文复制引用
刘永涛,董靖,杨秋红,余琳雪,杨移斌,何力,艾晓辉..改良的QuEChERS与HPLC-HESI/MS/MS同时测定中华鳖组织中氯硝柳胺和酰胺醇类药物及其代谢物的残留量[J].分析测试学报,2017,36(8):955-962,8.基金项目
中国水产科学研究院基本科研业务费资助项目(2016JBF0104) （2016JBF0104）
现代农业人才支撑计划项目(2016-2020) （2016-2020）
