采用液相色谱-电喷雾电离-串联质谱法和四极杆飞行时间质谱法对54个样品中的11种促智化合物进行了同时检测和分析

IF 1.3 Q4 CHEMISTRY, ANALYTICAL
Nam Sook Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Hyungil Kim, Sooyeul Cho
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引用次数: 0

摘要

用于改善大脑功能和增强注意力的膳食补充剂越来越受欢迎。然而,含有未经批准药物的非法膳食补充剂继续被查获。因此,为了公共安全,有必要快速筛选和鉴定膳食补充剂中的掺假化合物。为了建立同时分析方法,我们选择了11种益智药化合物,并对液相色谱-电喷雾电离-串联质谱法进行了优化,并提出了液相色谱-四极杆飞行时间质谱法的最佳条件,以确定每种化合物的破碎模式。根据国际验证指南对该方法的特异性、线性度、检出限、定量限、方法检出限、方法定量限、精密度、准确度、基质效应、稳定性进行评价。将验证的方法应用于54份含有膳食补充剂的样品和查获的样品。通过筛选,在4种固体样品(片剂和粉剂)中检出11种促智化合物。通过与标准品和定量品的离子比比较,3个样品中检出长春西汀(6.52 ~ 34.2 mg/g), 1个样品中检出昂贝西坦(995.6 mg/g)。为了重新确认检测到的化合物,使用液相色谱-四极杆飞行时间质谱法将碎片模式与标准品的碎片模式进行比较。所开发的同步分析方法有助于维护公共卫生和安全。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Simultaneous detection and analysis of 11 nootropic compounds in 54 samples via liquid chromatography‐electrospray ionization‐tandem mass spectrometry and quadrupole time‐of‐flight mass spectrometry
Abstract Dietary supplements used for improving brain function and strengthening attention are increasingly popular. However, illegal dietary supplements containing unapproved drugs continue to be seized. Therefore, it is necessary to rapidly screen and identify adulterated compounds in dietary supplements for public safety. To develop the simultaneous analytical method, we selected 11 nootropic compounds and optimized the simultaneous liquid chromatography‐electrospray ionization‐tandem mass spectrometry and optimal conditions for liquid chromatography‐quadrupole time‐of‐flight mass spectrometry were proposed to determine the fragmentation patterns of each compound. The specificity, linearity, limit of detection, limit of quantification, method detection limit, method quantitation limit, precision, accuracy, matrix effect, and stability of this method were evaluated according to international validation guidelines. The validated methods were applied to 54 samples containing dietary supplements and seized samples. On screening 11 nootropic compounds were detected in four solid samples (tablet and powder). By comparing the product ion ratios with the standards and quantification, vinpocetine (6.52–34.2 mg/g) was found in three samples, and omberacetam (995.6 mg/g) in one sample. To re‐confirm the detected compounds, the fragmentation patterns were compared with those of the standards using liquid chromatography‐quadrupole time‐of‐flight mass spectrometry. The developed simultaneous analysis method can help maintain public health and safety.
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来源期刊
SEPARATION SCIENCE PLUS
SEPARATION SCIENCE PLUS CHEMISTRY, ANALYTICAL-
CiteScore
1.90
自引率
9.10%
发文量
111
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