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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,C_(18)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0.4~10μg/kg和0.5~10μg/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0.4μg/kg和0.5μg/kg;HPLC-MS/MS方法在0.4、5和10μg/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5μg/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 and analyze the content of estradiol in aquatic products by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and gas chromatography-mass spectrometry (GC-MS) Alcohol residue. Methods HPLC-MS / MS method: The estradiol in the sample was extracted by methanol-water solution, and purified by solid-phase extraction. The content of estradiol was determined by HPLC-MS / MS and quantified by internal standard method. GC- Under acidic condition, the estradiol in the sample was extracted with acetonitrile, purified by C 18 column, derivatized with silylating reagent, and then determined by GC-MS and quantified by internal standard method. Results There was a good linear relationship between HPLC-MS / MS and GC-MS in the concentration range of 0.4 ~ 10μg / kg and 0.5 ~ 10μg / kg, the correlation coefficients were 0.9996 and 0.9994, kg and 0.5 μg / kg, respectively. The recoveries of HPLC-MS / MS at the spiked levels of 0.4, 5 and 10 μg / kg ranged from 88.81% to 106.0% with the precision of 2.5% to 6.5% And 5μg / kg added level of recovery was 80.24% ~ 96.60%, the precision of 1.4% ~ 5.4%. Conclusion The two detection methods have good linearity, both of them can be quantitatively and qualitatively determined. However, HPLC-MS / MS has lower detection limit and higher sensitivity, and the pretreatment method is more convenient, time-saving and efficient, which can effectively improve the detection efficiency of estradiol residues in aquatic products, save the testing cost, Product quality monitoring and testing provides a technical reference.