State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China.
Division of Metrology in Chemistry, National Institute of Metrology, Beijing 100013, China.
Talanta. 2014 Mar;120:248-54. doi: 10.1016/j.talanta.2013.11.086. Epub 2013 Dec 6.
A new method for the simultaneous determination of 7 synthetic musks (musk amberette, musk tibetene, musk moskene, musk ketone, musk xylene, phantolide, and tonalide) in cream by means of supporting liquid extraction (SLE) coupled with LC-Alumina-N SPE, then followed by GC-MS/MS has been established. In this study, 7 synthetic musks are extracted and pre-purified by a mixture solution of water and isopropanol from cream, and separated and purified by tandem columns containing SLE column and LC-Alumina-N SPE column, which were seldom reported before. Ultrasonic and mechanical shaking were applied to improve the extraction efficiency. Different experiment conditions, such as the type of extraction solution, extraction time of ultrasonic and mechanical shaking, the type of SLE and SPE column, and matrix effects were optimized and the recoveries of 7 synthetic musks for each part were above 86.61%. In addition, the use of isotope internal standards was systemically discussed. The method showed satisfactory linearity over the range assayed (5-1000 ng g(-1)), and the limits of detections (LODs) ranged from 0.15 to 4.86 ng g(-1), and the limits of quantifications (LOQs) were ranging from 0.49 to 16.21 ng g(-1). The recoveries using this method at three spiked concentration levels (10, 100, and 1000 ng g(-1)) range from 85.6% to 109%. The relative standard deviation was lower than 9.8% in all case. The proposed analytical method has been successfully applied for the analysis of 7 synthetic musks in commercial cream.
建立了一种新的方法，通过支持液萃取（SLE）与 LC-氧化铝-N SPE 联用，从乳膏中提取和预纯化 7 种合成麝香（琥珀麝香、西藏麝香、麝香酮、麝香二甲苯、磷苯甲酮、麝香环十五内酯和麝香桃醛），然后用 GC-MS/MS 进行分析。在本研究中，7 种合成麝香从乳膏中用异丙醇和水的混合溶液提取，然后通过串联的 SLE 柱和 LC-氧化铝-N SPE 柱进行分离和纯化，这在以前的研究中很少报道。采用超声和机械振荡来提高提取效率。优化了不同的实验条件，如提取溶液的类型、超声和机械振荡的提取时间、SLE 和 SPE 柱的类型以及基质效应等，7 种合成麝香的各部分回收率均高于 86.61%。此外，还系统地讨论了同位素内标物的使用。该方法在测定范围内（5-1000 ng g(-1))表现出令人满意的线性关系，检测限（LOD）范围为 0.15-4.86 ng g(-1)，定量限（LOQ）范围为 0.49-16.21 ng g(-1)。该方法在 3 个加标浓度水平（10、100 和 1000 ng g(-1))的回收率在 85.6%-109%之间。在所有情况下，相对标准偏差均低于 9.8%。该分析方法已成功应用于商业乳膏中 7 种合成麝香的分析。
