超高效液相色谱-串联质谱法同时测定清咽类保健食品中14种β2-受体激动剂非法添加物
目的 建立超高效液相色谱-串联质谱法同时测定清咽类保健食品中非法添加的14种β2-受体激动剂含量的分析方法。方法 样品经乙酸钠-甲醇混合溶液提取, 用氢氧化钠溶液调节pH值, 待测物由二氯甲烷-乙酸乙酯混合溶剂液液萃取, 经阳离子固相萃取小柱富集、净化后, 采用C18色谱柱分离, 以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱, 采用正离子多反应离子检测模式对14种β2-受体激动剂的含量进行检测, 内标法定量。结果 14种β2-受体激动剂在0.5~20 ng/mL(1.0~40 μg/kg)范围内线性关系良好, 相关系数均大于0.99。各待测物方法定量限为1.0 μg/kg。加标回收率为75.9%~110.9%, 相对标准偏差为1.9%~9.7%。结论 该方法准确、灵敏, 适用于清咽类保健食品中14种β2-受体激动剂的测定。
Objective To establish a method for the simultaneous determination of the content of 14 kinds of β2-agonists illegally added to Qingyan health food by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted by the mixed solution of sodium acetate and methanol, and the pH value was adjusted by sodium hydroxide solution. The analyte was extracted with dichloromethane-ethyl acetate mixed solvent liquid-liquid, enriched and purified by cationic solid phase extraction cartridge, separated by C18 column using acetonitrile and 0.1% formic acid aqueous solution as mobile phase for gradient elution. The content of 14 β2-agonists was determined by using the positive ion multiple reaction ion detection mode, and quantified by internal standard method. Results The 14 β2-receptor agonists had good linear relationship in the range of 0.5?20 ng/mL (1.0?40 μg/kg), and the correlation coefficients were all greater than 0.99. The limit of quantification of each analyte method was 1.0 μg/kg. The standard recoveries were 75.9%?110.9%, and the relative standard deviations were 1.9%?9.7%. Conclusion This method is accurate, sensitive and suitable for the determination of 14 β2 agonists in Qingyan health food.
标题：超高效液相色谱-串联质谱法同时测定清咽类保健食品中14种β2-受体激动剂非法添加物
英文标题：Simultaneous determination of 14 illegal β2-agonist additives in Qingyan health food by ultra performance liquid chromatography-tandem mass spectrometry
作者：
郭建博 陕西省食品药品监督检验研究院
薛晓文 陕西省食品药品监督检验研究院
刘开 陕西省食品药品监督检验研究院
宋莉 陕西省食品药品监督检验研究院
王蕊 陕西省食品药品监督检验研究院
林芳 陕西省食品药品监督检验研究院
王晶 陕西省食品药品监督检验研究院
李涛 陕西省食品药品监督检验研究院
中文关键词:β2-受体激动剂,超高效液相色谱-串联质谱法,清咽类保健食品,非法添加,
英文关键词:β2-agonist,ultra performance liquid chromatography tandem mass spectrometry,Qingyan health food,illegal addition,
发表日期：2020-07-23
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