高效液相色谱-串联质谱法同时测定鸡蛋中头孢噻肟及其主要代谢物残留

发布时间：2018-07-06 12:00

本文选题：鸡蛋 + 头孢噻肟　；参考：《分析化学》2017年07期

【摘要】：建立了高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定鸡蛋中头孢噻肟及其代谢物去乙酰头孢噻肟残留量的检测方法。样品经乙腈-水(9∶1,V/V)提取,正己烷除脂,C_(18)固相分散萃取除杂,Agilent Eclipse Plus C_(18)色谱柱(100 mm×2.1 mm,3.5μm)分离,以0.2%(V/V)甲酸-乙腈为流动相,进行梯度洗脱,目标物采用电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。结果表明,头孢噻肟和去乙酰头孢噻肟分别在1.0~143.0μg/L和1.0~120.0μg/L浓度范围内线性关系良好(R~20.999)。方法检出限(LOD,S/N=3)分别为0.07和0.14μg/kg,定量限(LOQ,S/N=10)分别为0.23和0.99μg/kg。在5.0、50.0和100.0μg/kg 3个添加水平下,头孢噻肟和去乙酰头孢噻肟的回收率分别为83.1%~103.0%和88.2%~101.0%,相对标准偏差(RSD,n=6)均介于2.0%~6.2%。实际样品测定结果表明,本方法简便、快速、灵敏、准确,可用于鸡蛋中头孢噻肟及去乙酰头孢噻肟的残留分析检测。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed for the simultaneous determination of cefotaxime and its metabolite deacetyl cefotaxime in eggs. The sample was extracted by acetonitrile-water (9: 1 V / V), n-hexane degreasing C _ (18) was separated by solid phase dispersion extraction (Agilent Eclipse Plus C _ (18) column (100 mm 脳 2.1 mm ~ (3.5 渭 m), the mobile phase was 0.2% (V / V) formic acid-acetonitrile, and the target was ionized by electrospray positive ion (ESI) mode. Multiple reaction monitoring (MRM) mode detection, matrix matching standard solution external standard method quantitative. The results showed that the linear range of cefotaxime and deacetyl cefotaxime was 1.0 渭 g / L and 1.0 渭 g / L, respectively (RV 20.999). Methods the detection limits (LOD) were 0.07 and 0.14 渭 g / kg, and the quantitative limits were 0.23 and 0.99 渭 g / kg, respectively. The recoveries of cefotaxime and deacetyl cefotaxime were 83.1103.0% and 88.2101.0%, respectively, and the relative standard deviations (RSD) were between 2.0 and 6.2. 2 at the addition level of 5.0 渭 g/kg and 100.0 渭 g/kg, the recoveries of cefotaxime and deacetyl cefotaxime were 83.1% and 88.2%, respectively. The results showed that the method was simple, rapid, sensitive and accurate, and could be used for the determination of cefotaxime and deacetyl cefotaxime in eggs.
【作者单位】：中国农业科学院农业质量标准与检测技术研究所农业部农产品质量安全重点实验室;南京农业大学食品科技学院肉品加工与质量控制教育部重点实验室;
【基金】：中国农业科学院科技创新工程项目资助
【分类号】：O657.63;TS253.7

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