Beijing Research Center for Preventive Medicine, Beijing 100013, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 1;879(21):1861-9. doi: 10.1016/j.jchromb.2011.04.036. Epub 2011 May 7.
A comprehensive method was developed for the simultaneous analysis in human breast milk of 12 synthetic musks, five nitro musks, six polycyclic muks and one macrocyclic musk; as well as one musk metabolite and triclosan. The target analytes were freeze dried and extracted using the accelerated solvent extraction (ASE) procedure. The extracts were further purified by gel permeation chromatography (GPC) and florisil solid-phase extraction (SPE) and then analyzed by gas chromatography tandem mass spectrometry (GC-MS/MS). Recoveries of the analytes based on the isotopic internal standard correction ranged from 82.4% to 112%, with relative standard derivations less than 20%. The method quantification limits (MQLs) were 0.6-5.4 ng/g lipid. The analytes were detected in human breast milk samples and ranged from 11.7 to 308.6 ng/g lipid.
建立了一种同时分析人乳中 12 种合成麝香、5 种硝基麝香、6 种多环麝香和 1 种大环麝香;以及 1 种麝香代谢物和三氯生的综合方法。采用加速溶剂萃取(ASE)程序对目标分析物进行冷冻干燥和提取。提取液进一步通过凝胶渗透色谱(GPC)和 Florisil 固相萃取(SPE)进行纯化,然后通过气相色谱串联质谱(GC-MS/MS)进行分析。基于同位素内标校正的分析物回收率在 82.4%至 112%之间,相对标准偏差小于 20%。方法定量限(MQLs)为 0.6-5.4ng/g 脂质。在人乳样中检测到这些分析物,其浓度范围为 11.7-308.6ng/g 脂质。