Lee Ji Hyun, Park Han Na, Kim Nam Sook, Park Seongsoo, Lee Yong-Moon, Kang Hoil
Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea.
College of Pharmacy, Chungbuk National University, Cheongju-si, Chungcheongbuk-do 28159, Republic of Korea.
Sci Justice. 2020 Jan;60(1):86-94. doi: 10.1016/j.scijus.2019.08.001. Epub 2019 Aug 13.
Over the past decade, illicit drugs have been founded in marketed products, which pose a risk to public health. In particular, newly designed analogues synthesized by chemical modification of parent compounds to avoid detection by authorities are frequently detected worldwide. Although many analytical methods for determination of drugs have been reported, analytical methods using high-resolution mass spectrometry, which has the advantage of rapid screening and accurate identification of new substances, are necessary to control illicit drugs in marketed products. In this study, a rapid analytical method using an Orbitrap™ mass spectrometer for identification of illicit drugs in marketed products was developed. The 32 drugs were classified as benzodiazepine-, synthetic cannabinoid-, amphetamine- and benzylpiperazine-type drugs according to their chemical structures, and from their fragmentation patterns in tandem mass spectrometry spectra of an established method. The method validation gave a limit of detection of 0.06-5.30 ng/mL and a limit of quantification of 0.18-16.50 ng/mL, high linearity (R > 0.994) and mean recoveries of spiked matrix-blank samples ranging from 83.7% to 117.1%. Approximately 71% of 21 samples collected over 3 years were found to individually contain one of four types of benzodiazepines or two different synthetic cannabinoids. In one case, levels as high as 827.2 mg/g were measured suggesting adulteration at high levels, which suggests that potential illicit products containing drugs should be regularly screened to protect public health.
在过去十年中,市售产品中发现了非法药物,这对公众健康构成了风险。特别是,通过对母体化合物进行化学修饰以避免被当局检测到而新设计的类似物在全球范围内经常被检测到。尽管已经报道了许多测定药物的分析方法,但为了控制市售产品中的非法药物,仍需要使用高分辨率质谱的分析方法,该方法具有快速筛查和准确鉴定新物质的优势。在本研究中,开发了一种使用Orbitrap™质谱仪鉴定市售产品中非法药物的快速分析方法。根据其化学结构以及既定方法的串联质谱图中的碎片模式,将这32种药物分为苯二氮䓬类、合成大麻素类、苯丙胺类和苄基哌嗪类药物。方法验证得出检测限为0.06 - 5.30 ng/mL,定量限为0.18 - 16.50 ng/mL,线性良好(R > 0.994),加标基质空白样品的平均回收率在83.7%至117.1%之间。在三年间收集的21个样品中,约71%被发现分别含有四种苯二氮䓬类药物中的一种或两种不同的合成大麻素。在一个案例中,测得的含量高达827.2 mg/g,表明存在高剂量掺假,这表明应定期筛查含有药物的潜在非法产品以保护公众健康。