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Ultrasound-assisted emulsification microextraction for rapid determination of unmetabolized synthetic polycyclic and nitro-aromatic musks in human urine
Journal of Chromatography B ( IF 2.8 ) Pub Date : 2018-06-20 , DOI: 10.1016/j.jchromb.2018.06.042
Ting-An Chen , Wu-Hsun Chung , Erica M.C. Ding , Wang-Hsien Ding

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.



中文翻译:

超声辅助乳化微萃取快速测定人尿中未代谢的合成多环和硝基芳族麝香

开发了一种快速测定人尿液样品中七个未代谢合成麝香的有效方法。目标麝香是五种合成的多环麝香(即塞莱斯托利德(ADBI),杀螨醇(AHMI),曲沙奈德(ATII),galaxolide(HHCB),托纳利德(AHTN))和两只硝基芳族麝香(即麝香二甲苯(MX )和麝香酮(MK))。该方法包括超声辅助乳化微萃取(USAEME)和气相色谱-质谱(GC-MS)。对影响USAEME效率的因素进行了详细优化,优化程序包括将50μL四氯化碳快速注入锥形底玻璃管中的1.0 mL尿液样本(含0.1 g氯化钠)中。超声处理1.0分钟并离心3分钟(7000 rpm)后,将沉淀的提取物10μL直接注入GC-MS系统。定量限(LOQ)从0.1到0.5 ng / mL不等。重复性和再现性的精度均小于8%。真实度从79%到96%不等,RSD从2%到8%不等。收集的人类尿液样本中的七个未代谢的目标麝香的总浓度在0.93至3.74 ng / mL的范围内。在所有收集的样品中都检测出六六六和AHTN,并对每日排泄剂量进行了评估。收集的人类尿液样本中的七个未代谢的目标麝香的总浓度在0.93至3.74 ng / mL的范围内。在所有收集的样品中都检测出六六六和AHTN,并对每日排泄剂量进行了评估。收集的人类尿液样本中的七个未代谢的目标麝香的总浓度在0.93至3.74 ng / mL的范围内。在所有收集的样品中都检测出六六六和AHTN,并对每日排泄剂量进行了评估。

更新日期:2018-06-20
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