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采用基质固相分散萃取结合超高压液相色谱-串联质谱法分析鸡蛋中的八种游离孕激素。

Analysis of eight free progestogens in eggs by matrix solid-phase dispersion extraction and very high pressure liquid chromatography with tandem mass spectrometry.

作者信息

Yang Yi, Shao Bing, Zhang Jing, Wu Yongning, Ying Jie

机构信息

Central Lab, Beijing Center for Disease Control and Prevention, Beijing 100013, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Jul 15;870(2):241-6. doi: 10.1016/j.jchromb.2008.06.021. Epub 2008 Jun 20.

Abstract

A rapid method to identify and quantify unconjugated progestogens in eggs is presented. Samples were prepared based on matrix solid-phase dispersion (MSPD) using C18 as dispersant, followed by a clean-up step with graphitized carbon black (GCB) solid-phase extraction (SPE) cartridges. The analytes were separated by very high pressure LC on a BEH C18 column for a period of 5 min. Electrospray ionization tandem mass spectrometry (ESI-MS/MS) was operated in the positive time-scheduled multi-reaction monitoring mode. Recovery studies were performed at two fortification levels. Average recoveries of the target compounds varied from 83.8% to 111.2% and relative standard deviations ranged from 10.5% to 23.7%. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.2-2.0 microg kg(-1) and 0.6-5.0 microg kg(-1), respectively. Investigation of real samples indicated that the range of progesterone in eggs was 9.9-40.0 microg kg(-1).

摘要

本文介绍了一种快速鉴定和定量鸡蛋中未结合孕激素的方法。样品基于基质固相分散(MSPD)制备,使用C18作为分散剂,随后用石墨化炭黑(GCB)固相萃取(SPE)小柱进行净化步骤。分析物在BEH C18柱上通过超高压液相色谱分离5分钟。电喷雾电离串联质谱(ESI-MS/MS)在正离子定时多反应监测模式下运行。在两个加标水平上进行了回收率研究。目标化合物的平均回收率在83.8%至111.2%之间,相对标准偏差在10.5%至23.7%之间。检测限(LOD)和定量限(LOQ)分别在0.2 - 2.0微克/千克和0.6 - 5.0微克/千克范围内。实际样品调查表明,鸡蛋中孕酮的含量范围为9.9 - 40.0微克/千克。

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