Yang Yi, Shao Bing, Zhang Jing, Wu Yongning, Ying Jie
Central Lab, Beijing Center for Disease Control and Prevention, Beijing 100013, China.
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.
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).
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。
