摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定水产品中17α-雌二醇与17β-雌二醇的方法。方法样品经水-乙腈(2:8,V:V)提取,加入N-丙基乙二胺、C18、中性氧化铝进行净化,提取液氮吹至干,残渣用水-乙腈(8:2,V:V)溶解。样液以水-乙腈(均含5 mmol/L氨水)为流动相,经C18色谱柱分离后进行多反应监测(multiple reaction monitoring,MRM)模式的定性及定量分析,外标法定量。结果17α-雌二醇与17β-雌二醇在质量浓度5~200μg/L范围内线性良好,相关系数分别为0.9998和0.9985;3个加标水平的平均回收率为66.5%~101.1%,相对标准偏差为0.62%~10.17%;检出限范围为0.85~0.90μg/kg,定量限范围为2.1~2.4μg/kg。结论该方法操作简单快捷、灵敏准确,适用于鱼、虾、蟹、贝等水产品中17α-雌二醇与17β-雌二醇的定性及定量分析。
Objective To establish a method for the determination of 17α-estradiol and 17β-estradiol in aquatic products by QuEChERS combined with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample was extracted with water-acetonitrile(2:8,V:V),purified with N-propylethylenediamine,C18 and neutral alumina,blown to dryness with nitrogen,and then reconstituted with water-acetonitrile(8:2,V:V).The sample solution was analyzed using water and acetonitrile(both containing 5 mmol/L ammonia)as mobile phase,separated by C18 chromatographic column,scanned and detected in multiple reaction monitoring(MRM)mode,and quantified by external standard method.Results The results showed that 17α-estradiol and 17β-estradiol showed a good linear relationship in the concentration ranges of 5 to 200μg/L,and the correlation coefficients were 0.9998 and 0.9985,respectively.The average recoveries at three spiked concentration levels varied from 66.5%to 101.1%with relative standard deviations of 0.62%to 10.17%.The limit of detection was 0.85–0.90μg/kg,and the limit of quantitation was 2.1–2.4μg/kg.Conclusion This method is simple,fast,sensitive and accurate,suitable for qualitative and quantitative analysis of 17α-estradiol and 17β-estradiol in aquatic products such as fish,shrimp,crabs and shellfish.
作者
肖明昊
袁梓洢
李诗婷
梁静
汪苹
杨悦
吴济舟
XIAO Ming-Hao;YUAN Zi-Yi;LI Shi-Ting;LIANG Jing;WANG Ping;YANG Yue;WU Ji-Zhou(China Testing Holding Group Jingcheng Testing Co.,Ltd.,Guangzhou 511400,China;China Testing Holding Group Beijing Ecological Environmental Protection Technology Research Institute Co.,Ltd.,Beijing 100024,China)
出处
《食品安全质量检测学报》
2025年第16期67-74,共8页
Journal of Food Safety and Quality
基金
2023年度国检科研基金项目(GJ012023078)。
关键词
超高效液相色谱-串联质谱法
水产品
雌二醇
QUECHERS
ultra performance liquid chromatography-tandem mass spectrometry
aquatic products
estradiol
QuEChERS
