超高压液相色谱-串联质谱法检测猪肉中玉米赤霉醇类物质

Simultaneous determination of zeranol and related analogues in pork by ultra pressure liquid chromatography-tandem mass spectrometry

中文关键词:  超高压液相色谱-串联质谱(UPLC-MS/MS)  玉米赤霉醇  固相萃取  猪肉

英文关键词:ultra pressure liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  zeranol and related analogues  solid-phase extraction(SPE)  pork

中文摘要:

      目的 建立猪肉中6种玉米赤霉醇类物质(α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮)的超高压液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法 样品经β-葡萄糖苷酶/硫酸酯酶酶解, 无水乙醚萃取, 再经氢氧化钠溶液液-液分配, 最后通过HLB固相萃取柱富集净化, UPLC-MS/MS检测, 基质匹配外标标准曲线法定量。结果 6种玉米赤霉醇类物质的线性范围为1.0~250 μg/L, 相关系数r＞0.990。当取样量为5.0 g时, 6种玉米赤霉醇类物质检出限为0.4 μg/kg。3个不同水平(添加1.0、5.0、20 μg/kg)的加标平均回收率为66.0%~79.5%, 相对标准偏差不大于10%。结论 所建立的方法具有较好的回收率和精密度, 准确度和灵敏度高, 符合猪肉中玉米赤霉醇类物质痕量的检测要求, 为大通量样品的食品安全检测提供更灵敏、高效的技术支持。

英文摘要:

      Objective To establish an ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of zeranol and related analogues(α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalanone and zearalenone) in pork. Methods After β-gluco-sidase/sulfatase enzymolysis, the samples were extracted by diethyl ether anhydrous, followed by liquid-liquid extraction with sodium hydrate solution, finally enriched and purified by HLB solid-phase extraction cartridge, and determined by UPLC-MS/MS, quantified by matrix matched external standard method. Results The calibration curves of the 6 compounds showed a good linearity between the peak areas and the concentrations of 1.0～250 μg/L with r > 0.990. The limits of detection of the 6 compounds were 0.4 μg/kg. The mean recoveries of the 6 compounds ranged from 66.0% to 79.5% spiked at three concentration levels (add 1.0, 5.0 μg/kg and 20 μg/kg), with the relative standard deviations (RSD) less than 10%. Conclusion The established method has good recovery and precision, high accuracy and sensitivity, and comply with the regulations for the determination of zeranol and related analogues trace contaminants residues in pork, provided more sensitive and efficient technical support of the large throughput sample for food safety determination.