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

Determination of Prostaglandin E2 in Pork and Lymph Nodes by Ultra-Performance Liquid Chromatography-tandem Mass Spectrometry

摘要:

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。

Abstract:

A method was developed for the determination of prostaglandin E2 in pork and lymph nodes based on ultraperformance 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.