超高效液相色谱-串联质谱法测定猪肉和淋巴肉中前列腺素E2含量OA北大核心CSTPCD
Determination of Prostaglandin E2 in Pork and Lymph Nodes by Ultra-Performance Liquid Chromatography-tandem Mass Spectrometry
该文建立了基于超高效液相色谱-串联质谱测定猪肉和淋巴肉中前列腺素E2 含量的方法.猪肉及淋巴肉样品经乙腈提取,乙腈饱和的正己烷除脂,HLB固相萃取柱净化,洗脱液于 45℃下用氮气吹至近干,φ=50%乙腈水(含 0.2%甲酸)溶液复溶后测定.以 0.1%甲酸溶液和乙腈为流动相,采用C18 色谱柱分离,负离子模式进行多反应监测.猪肉及其制品中前列腺素E2 的检出限为 10 μg/kg,定量限为 20 μg/kg.方法中前列腺素E2 回收率在 90%~120%范围内,精密度小于 15.0%,方法的准确度和精密度均满足定量分析的要求.利用所建立的方法测定实际样本,非淋巴肉样本中前列腺素E2 的本底值低于定量限,淋巴肉样本中前列腺素E2 的含量范围为20.7~101.0 μg/kg,通过测定样本中前列腺素E2 的含量可作为鉴别淋巴肉的一种辅助手段.该方法准确度高,可推广性强,为打击淋巴肉违法使用提供有力的技术支撑.
A method was developed for the determination of prostaglandin E2 in pork and lymph nodes based on ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were extracted with acetonitrile,defatted with acetonitrile-saturated n-hexane,cleaned up by HLB solid-phase extraction columns,and the eluates were blown to near-dryness with nitrogen at 45℃and determined by re-solubilizing in a 50%acetonitrile solution containing 0.2%formic acid.The separation was conducted on a C18 column with 0.1%formic acid solution and acetonitrile as mobile phases,and the multiple reaction monitoring was performed in negative ion mode.The limit of detection for prostaglandin E2 in pork and its products was 10 μg/kg,and the limit of quantification was 20 μg/kg.The recoveries of prostaglandin E2 in the method were in the range of 90~120%,and the precision was below 15.0%.The accuracy and precision of the method met the requirements for quantitative analysis.The values of prostaglandin E2 in non-lymph node samples were below the limit of quantification using the established method,and the range of prostaglandin E2 in lymph node samples was 20.7~101.0 μg/kg.By determining the amount of prostaglandin E2 in a sample,it can be used as an aid in identifying lymph nodes.This method is highly accurate and generalizable,and it provides strong technical support for combating the illegal use of lymph nodes.
汪薇;吴婉琴;江丰;朱晓玲;张莉
湖北省食品质量安全监督检验研究院,国家市场监管重点实验室(动物源性食品中重点化学危害物检测技术),湖北省食品质量安全检测工程技术研究中心,湖北武汉 430075
前列腺素E2淋巴肉猪肉及其制品质谱
prostaglandin E2lymph nodespork and its productsmass spectrometry
《现代食品科技》 2024 (007)
276-285 / 10
国家市场监督管理总局科技计划项目(2021MK070);国家重点研发计划(2018YFC1602303).
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