Research Center for Environmental Changes, Academia Sinica, Nankang, Taipei, Taiwan 115.
Anal Chem. 2011 Jun 15;83(12):4955-61. doi: 10.1021/ac2006872. Epub 2011 May 17.
The occurrence and potential toxicity of synthetic musks in environmental media have aroused concerns for the impacts of these chemicals on ecosystems and human health. Here, we present the first method using ultra-performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry (UPLC-APPI-MS/MS) for analysis of the six most important synthetic musks. Analysis was performed on an API 3000 triple quadrupole equipped with a PhotoSpray APPI source. Two pairs of precursor/product ions are presented that are essential for confirmation. Chromatographic separation is completed in 7 min in the positive mode and 5.1 min in the negative mode. Furthermore, three dopant solutions (0.5% anisole in toluene, 0.5% 2,4-difluoroanisole (DFA) in bromobenzene, and 0.5% DFA in chlorobenzene) are compared in terms of sensitivity, linearity, precision, and accuracy. The best sensitivity is associated with 0.5% anisole in toluene as the dopant; all LODs are below 6 pg. The linear range is 5 to 500 ppb with fairly good precision and accuracy. This analytical method has also proven its applicability by analyzing real air samples. In summary, we present a fast, sensitive, and reliable UPLC-APPI-MS/MS method for six important synthetic musks; it can be readily applied to environmental studies.
合成麝香在环境介质中的出现及其潜在毒性引起了人们对这些化学物质对生态系统和人类健康影响的关注。在这里,我们首次提出了一种使用超高效液相色谱-大气压光电离串联质谱(UPLC-APPI-MS/MS)分析六种最重要的合成麝香的方法。分析在配备 PhotoSpray APPI 源的 API 3000 三重四极杆上进行。提出了两对用于确证的前体/产物离子对。在正模式下,色谱分离在 7 分钟内完成,在负模式下,5.1 分钟内完成。此外,还比较了三种掺杂溶液(甲苯中的 0.5%苯甲醚、溴苯中的 0.5%2,4-二氟苯甲醚(DFA)和氯苯中的 0.5%DFA)在灵敏度、线性度、精密度和准确性方面的性能。灵敏度最好的是甲苯中的 0.5%苯甲醚作为掺杂剂;所有的检出限都低于 6 皮克。线性范围为 5 至 500 ppb,具有相当好的精密度和准确性。该分析方法还通过分析实际空气样本证明了其适用性。总之,我们提出了一种快速、灵敏、可靠的 UPLC-APPI-MS/MS 方法,用于分析六种重要的合成麝香;它可以很容易地应用于环境研究。