Choi Ji Yeon, Heo Seok, Yoo Geum Joo, Park Sung-Kwan, Yoon Chang-Yong, Baek Sun Young
a Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong Health Technology Administration Complex , Heungdeok-gu , Cheongju-si , Korea.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2015;32(7):1029-39. doi: 10.1080/19440049.2015.1040080. Epub 2015 May 26.
The purpose of this study was to develop a method to analyse the concentration of multiple illegal narcotics present in dietary supplements. To this end, we established and optimised a procedure using LC-MS/MS simultaneously to analyse 28 narcotic compounds in various forms of dietary supplements, including powders, tablets, liquids and capsules. In addition, candy and cookies that have also had detected cases of adulteration were also analysed. The specificity, linearity, accuracy, precision, limit of detection (LOD), limit of quantitation (LOQ), stability and recovery for these methods were validated accordingly. The LOD and LOQ of the LC-MS/MS ranged from 0.01-50.0 to 0.03-100 ng g(-1), respectively. The linearity of these results was good (r(2) > 0.99), with intra- and inter-day precision values of 0.2-5.2% and 0.2-4.8%, respectively. Further, the intra- and inter-day accuracies of this method were 97.0-103.4% and 94.6-103.1%, respectively. The stability RSD was less than 7.8%. The mean recovery for this LC-MS/MS procedure was 81.1-117.4%, with an RSD less than 9.8%. Following the validation of our method, we analysed 47 commercially available dietary supplements obtained in Korea. Whilst none of these samples had detectable amounts of the 28 specified narcotic adulterants, our novel LC-MS/MS procedure can be utilised comprehensively and continually to monitor illegal drug adulteration in various forms of dietary supplements.
本研究的目的是开发一种方法,用于分析膳食补充剂中多种非法麻醉药品的浓度。为此,我们建立并优化了一种程序,使用液相色谱-串联质谱法(LC-MS/MS)同时分析各种形式膳食补充剂(包括粉末、片剂、液体和胶囊)中的28种麻醉化合物。此外,还对已检测出掺假案例的糖果和饼干进行了分析。相应地验证了这些方法的特异性、线性、准确性、精密度、检测限(LOD)、定量限(LOQ)、稳定性和回收率。LC-MS/MS的LOD和LOQ分别为0.01 - 50.0 ng g(-1)和0.03 - 100 ng g(-1)。这些结果的线性良好(r(2) > 0.99),日内和日间精密度值分别为0.2 - 5.2%和0.2 - 4.8%。此外,该方法的日内和日间准确度分别为97.0 - 103.4%和94.6 - 103.1%。稳定性相对标准偏差(RSD)小于7.8%。该LC-MS/MS程序的平均回收率为81.1 - 117.4%,RSD小于9.8%。在我们的方法经过验证后,我们分析了在韩国获得的47种市售膳食补充剂。虽然这些样品中均未检测到28种指定的麻醉掺假物,但我们新颖的LC-MS/MS程序可被全面且持续地用于监测各种形式膳食补充剂中的非法药物掺假情况。