液质联用与气质联用测定水产品中雌二醇残留的方法比较
目的 比较分析高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)和气相色谱-质谱法(gas chromatography- mass spectrometry, GC-MS)测定水产品中雌二醇残留。方法 HPLC-MS/MS法: 样品中的雌二醇经酶解, 用甲醇-水溶液提取, 经固相萃取富集净化, 采用HPLC-MS/MS测定, 以内标法定量; GC-MS法: 酸性条件下, 以乙腈提取样品中的雌二醇, 经过正己烷脱脂, C18固相萃取柱净化, 硅烷化试剂衍生化后, 采用GC-MS测定, 以内标法定量。结果 HPLC-MS/MS和GC-MS分别在0.4~10 μg/kg和0.5~10 μg/kg浓度范围内有良好的线性关系, 相关系数r分别为0.9996和0.9994; 方法检出限分别为0.4 μg/kg和0.5 μg/kg; HPLC-MS/MS方法在0.4、5和10 μg/kg添加水平的回收率为88.81%~106.0%, 精密度为2.5%~6.5%; GC-MS方法在0.5、1和5 μg/kg添加水平的回收率为80.24%~96.60%, 精密度为1.4%~5.4%。结论 两种检测方法线性关系良好, 均可同时定量和定性。但HPLC-MS/MS降低了方法检出限, 灵敏度更高, 并且前处理方法更为简便、省时、高效, 可有效提高水产中雌二醇残留的检测效率, 节约检测成本, 并为水产品质量监控与检测提供了技术参考。
Objective To compare the detection methods of high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) for the determination of estradiol residues in aquatic products. Methods Samples for HPLC-MS/MS detection were extracted with methanol-water solution after enzymatic hydrolysis, cleaned up by solid-phase extraction, and then analyzed by HPLC-MS/MS and quantified by internal standard method. Meanwhile, the samples for GC-MS detection were extracted with acetonitrile under acidic condition, degreased by n-hexane, cleaned up by C18 solid phase extraction column before derviative reaction with silane agents, and finally quantified by internal standard method. Results The correlation coefficients of HPLC-MS/MS method and GC-MS method were respectively 0.9996 and 0.9994 in the corresponding concentration ranges of 0.4~10 μg/kg and 0.5~10 μg/kg, respectively. The limits of detection of HPLC-MS/MS method and GC-MS method were 0.4 μg/kg and 0.5 μg/kg, respectively. The mean recoveries of estradiol spiked at 3 levels of 0.4, 5, 10 μg/kg by HPLC-MS/MS method were within 88.81%~106.0% with relative standard deviations (RSD) of 2.5%~6.5%; while the mean recoveries of estradiol spiked at 3 levels of 0.5, 1, 5 μg/kg by GC-MS method were within 80.24%~96.60% with RSD of 1.4%~5.4%. Conclusion Two methods showed that estradiol had good linear relationships, which were suitable for quantitative and qualitative analysis. However, HPLC-MS/MS method has higher sensitivity and lower detection limit, with a more simple and efficient pretreatment, which can greatly increase the testing efficiency of estradiol residues in aquatic products and provide a reference for the quality and safety monitoring and detection of aquatic products.
标题：液质联用与气质联用测定水产品中雌二醇残留的方法比较
英文标题：Comparative study on the determination of estradiol residue in aquatic products by high performance liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry
作者：
张泸文 上海市食品药品检验所
王柯 上海市食品药品检验所
刘畅 上海市食品药品检验所
中文关键词:雌二醇,高效液相色谱-串联质谱法,气相色谱-质谱法,固相萃取,
英文关键词:estradiol,high performance liquid chromatography-tandem mass spectrometry,gas chromatography-mass spectrometry,solid-phase extraction,
发表日期：2016-06-03
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