串联固相萃取超高效液相色谱三重四极杆质谱法同时同时测定用于改善阳虚和/或缓解疲劳类的20种保健品非法添加物

Simultaneous determination of 20 kinds of illegally–added medicals in foods with claims of improving yang deficiency and/or relieving fatigue by series solid phase extraction–ultra performance liquid chromatography–triple quadrupole tandem mass spectrometry

中文关键词:  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

英文关键词:improving Yang deficiency  anti–fatigue preparations  series solid phase extraction  ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry  illegally added chemicals

中文摘要:

      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0.5~30 μg/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。

英文摘要:

      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.