论文部分内容阅读
目的:建立一种快速检测动物类药材污染黄曲霉毒素B_1(AFB_1)和G_1(AFC_1)的液质联用方法,并用于水蛭等6种动物类中药材污染情况的分析。方法:药材样品加84%乙腈提取,提取液挥干后用甲醇溶解,采用高效液相串联质谱法检测方法,C_(18)色谱柱(2.1 mm×100 mm,3μm),以甲醇-4.0 mmol-L~(-1)乙酸铵-0.1%甲酸水溶液为流动相梯度洗脱,质谱使用ESI离子源,正离子扫描模式,选择反应检测(SRM)模式进行定量。结果:6种药材中AFB.,AFC.的基质效应介于82%-119%;以水蛭作为代表性基质,进行添加回收率试验,按低、中、高3个浓度水平添加时,AFB,与AFC,的提取回收率、绝对回收率介于80%~117%,方法学考察精密度RSD 1.8%~7.5%,重复性RSD 5.1%~14%,将该方法应用于55份动物药材样品检测,结果显示包括水蛭和上鳖虫在内的4份样品受到污染,其中上鳖虫污染率达33.30%,污染水平为1.26~26.3μg·kg~(-1)。结论:上鳖虫等动物类药材受黄曲霉毒素污染的情况应当引起足够的重视。针对药材生产的各个环节,采取恰当的措施降低黄曲霉毒素污染的风险是十分必要的。
OBJECTIVE: To establish a liquid chromatography-mass spectrometry method for rapid detection of aflatoxins B_1 (AFB_1) and G_1 (AFC_1) in animal medicines, and to analyze the contamination of 6 kinds of Chinese herbal medicines such as leeches. METHODS: Medicinal samples were extracted with 84% acetonitrile and the extracts were evaporated to dryness and then dissolved in methanol. The compounds were separated on a C 18 column (2.1 mm × 100 mm, 3 μm) with methanol-4.0 mmol (-1) ammonium acetate-0.1% formic acid as mobile phase. The mass spectra were quantified using ESI source, positive ion scan mode and selective reaction detection (SRM) mode. Results: The matrix effects of AFB. And AFC in six medicinal herbs ranged from 82% to 119%. When leech was used as a representative matrix, the recoveries were tested at three concentration levels of AFB, The recoveries were in the range of 80% -117% with AFC. The methodological precision was 1.8% ~ 7.5% RSD and 5.1% ~ 14% RSD. The method was applied to 55 samples of animal medicine The results showed that 4 samples, including leeches and turtles, were contaminated. The contamination rate was 33.30% and the contamination level was 1.26 ~ 26.3 μg · kg -1. Conclusion: It is necessary to pay enough attention to the contamination of animal medicines such as beetles and insects by aflatoxins. For all aspects of the production of medicinal herbs, it is necessary to take appropriate measures to reduce the risk of aflatoxin contamination.