摘要
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0.5~20ng/mL(1.0~40μg/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1.0μg/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.
作者
郭建博
薛晓文
刘开
宋莉
王蕊
林芳
王晶
李涛
GUO Jian-Bo;XUE Xiao-Wen;LIU Kai;SONG Li;WANG Rui;LIN Fang;WANG Jing;LI Tao(Shaanxi Institute for Food and Drug Control,Xi’an 710065,China)
出处
《食品安全质量检测学报》
CAS
2020年第19期6767-6774,共8页
Journal of Food Safety and Quality
基金
陕西省重点产业链(群)项目(2019ZDLSF07-08)
陕西省创新能力支撑计划(2019PT-22)。
