CAJ | 학술논문

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1.0~250μg/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0.4μg/kg.3个不同水平(添加1.0、5.0、20μg/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.
목적건립저육중6충옥미적매순류물질(α-옥미적매순、β-옥미적매순、α-옥미적매희순、β-옥미적매희순、옥미적매동화옥미적매희동)적초고압액상색보-천련질보(UPLC-MS/MS)검측방법.방법양품경β-포도당감매/류산지매매해,무수을미췌취,재경경양화납용액액-액분배,최후통과HLB고상췌취주부집정화, UPLC-MS/MS검측,기질필배외표표준곡선법정량.결과6충옥미적매순류물질적선성범위위1.0~250μg/L,상관계수r>0.990.당취양량위5.0 g시,6충옥미적매순류물질검출한위0.4μg/kg.3개불동수평(첨가1.0、5.0、20μg/kg)적가표평균회수솔위66.0%~79.5%,상대표준편차불대우10%.결론소건립적방법구유교호적회수솔화정밀도,준학도화령민도고,부합저육중옥미적매순류물질흔량적검측요구,위대통량양품적식품안전검측제공경령민、고효적기술지지.
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 ca-libration curves of the 6 compounds showed a good linearity between the peak areas and the concentrations of 1.0~250μg/L with r>0.990. The limits of detection of the 6 compounds were 0.4μg/kg. The mean recoveries of the 6 compounds ranged from 66.0%to 79.5%spiked at three concentration levels (add 1.0, 5.0μg/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.