Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
Department of Chemical Engineering, Army Academy ROC, Chung-Li 320, Taiwan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Aug 15;1092:440-446. doi: 10.1016/j.jchromb.2018.06.042. Epub 2018 Jun 20.
An effective method to rapidly determine the presence of seven unmetabolized synthetic musks in human urine samples is developed. The target musks are five synthetic polycyclic musks (i.e., celestolide (ADBI), phantolide (AHMI), traseolide (ATII), galaxolide (HHCB), tonalide (AHTN)), and two nitro-aromatic musks (i.e., musk xylene (MX) and musk ketone (MK)). The method involved an ultrasound-assisted emulsification microextraction (USAEME) coupled with gas chromatography-mass spectrometry (GC-MS). The factors that affect USAEME efficiency were optimized in detail, and the optimized procedure involved the rapid injection of 50 μL of carbon tetrachloride into 1.0 mL of urine sample (contained 0.1-g of sodium chloride) in a conical bottom glass tube. After 1.0 min ultrasonication and 3 min centrifugation (at 7000 rpm), the sedimented extract 10 μL was directly injected into the GC-MS system. The limits of quantitation (LOQs) varied from 0.1 to 0.5 ng/mL. The precisions for both repeatability and reproducibility were <8%. The trueness varied from 79 to 96% with the RSD ranging from 2 to 8%. The total concentrations of the seven unmetabolized target musks in collected human urine samples were in the range from 0.93 to 3.74 ng/mL. HHCB and AHTN were detected in all the collected samples, and the daily excretion doses were evaluated.
建立了一种快速测定人尿样中七种未代谢合成麝香的有效方法。目标麝香为五种合成多环麝香（即 Celestolide (ADBI)、Phantolide (AHMI)、Traseolide (ATII)、Galaxolide (HHCB)、Tonalide (AHTN)）和两种硝基芳烃麝香（即 Musk Xylene (MX) 和 Musk Ketone (MK)）。该方法涉及超声辅助乳化微萃取（USAEME）与气相色谱-质谱联用（GC-MS）。详细优化了影响 USAEME 效率的因素，优化程序包括将 50 μL 四氯化碳快速注入锥形底玻璃管中 1.0 mL 尿液样品（含 0.1 g 氯化钠）。超声 1.0 分钟后，离心 3 分钟（7000 rpm），将沉淀的萃取物 10 μL 直接注入 GC-MS 系统。定量限（LOQ）范围为 0.1-0.5 ng/mL。重复性和再现性的精密度均<8%。准确度在 79-96%之间，相对标准偏差（RSD）在 2-8%之间。从收集的人尿样中，七种未代谢的目标麝香的总浓度范围为 0.93-3.74 ng/mL。所有收集的样品中均检测到 HHCB 和 AHTN，并对其日排泄剂量进行了评估。
