摘要
目的 建立串联式固相萃取–超高效液相色谱–三重四极杆质谱法(series solid phase extraction–ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry,SPE-UPLC-MS/MS)同时测定保健品中20种改善阳虚和/或缓解疲劳类化学物质的分析方法 .方法待测样品经预处理后,依次经过C18固相萃取柱、季胺固相萃取柱、羧酸固相萃取柱纯化.采用0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱,质谱(ESI+)采用多离子检测模式(multiple reaction monitoring,MRM)进行检测.结果 本方法在5 min内完成20种目标化合物的分离鉴定.20种改善阳虚或缓解疲劳类化合物在0.5~30μg/L浓度范围内呈良好的线性关系,相关系数(r)大于0.98,样品加标后平均回收率在82.0%~105.2%,相对标准偏差小于10%,方法定量限在0.1~0.5 ng/mL范围.结论 该方法快速、准确、灵敏度高且重现性好,为筛查改善阳虚和/或缓解疲劳类保健食品中非法添加物质提供有力工具.
Objective To establish a method for simultaneously determination of 20 kinds of yang-deficiency and/or fatigue-relieving chemicals in health food by series solid phase extraction-ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry(SPE-UPLC-MS/MS). Methods Samples were pretreated and purified via a series of solid phase extractions, including C18, SAX(quaternary amine), and WCX(carboxylic acid) SPE columns. And then samples were analyzed on a reversed phase using a gradient elution program of 0.1% formic acid aqueous solution(A) and 0.1% formic acid in acetonitrile solution(B), and determined using UPLC-MS/MS including electrospray ionization source and positive ion scan multiple reaction monitoring(MRM) mode. Results The isolation and identification of 20 target compounds were completed within 5 min. The results showed that 20 kinds medicals with functions of improving yang or relieving fatigue had good linear dose-response relationship in 0.5–30 μg/L, with correlation coefficients(r) greater than 0.98. The average yields were 82.0%–105.2%. The relative standard deviations(RSDs) were less than 10%, and the limits of quantitation(LOQ) for the 20 kinds medicals were between 0.1 and 0.5 ng/mL. Conclusion This method is rapid, accurate, sensitive and reproducible, which is a powerful tool to screen illegally medicals-added foods with claims of improving yang and/or relieving fatigue.
作者
谭丽容
程敏
林伟斌
张龙开
TAN Li-Rong;CHENG Min;LIN Wei-Bin;ZHANG Long-Kai(Hong Zheng Dao(China)Traditional Chinese Medicine Research Company Ltd.,Guangzhou 510665,China)
出处
《食品安全质量检测学报》
CAS
2019年第21期7418-7426,共9页
Journal of Food Safety and Quality
关键词
改善阳虚
缓解体力疲劳
固相萃取
超高效液相色谱-三重四极杆质谱法
非法添加物
improving Yang deficiency
anti-fatigue preparations
series solid phase extraction
ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry
illegally added chemicals
