摘要
目的:建立一种快速检测抗风湿类保健食品中5种Janus激酶(JAK)抑制药的分析方法。方法:采用液相色谱-串联四级杆质谱(LC-MS/MS),色谱柱:CAPCELL PAK C_(18)(3.0 mm×100 mm,3μm);流动相:0.1%甲酸乙腈(A)-0.1%乙酸溶液(B),梯度洗脱;流速:0.4 ml·min^(-1);柱温:35℃;电喷雾离子源(ESI),正离子采集模式,多反应检测模式(MRM)测定5种JAK抑制药,比较各通道对照品与样品的分子离子峰、碎片离子峰、色谱保留时间等信息确定非法添加的JAK抑制药种类。结果:5种JAK抑制药色谱分离良好,方法检出限为(LOD)0.02~0.21 ng·ml^(-1),定量限(LOD)为0.05~0.45 ng·ml^(-1),回收率在91.2%~102.9%。结论:该方法简单、准确,可用于保健食品中非法添加JAK抑制剂的检测。
Objective:To develop a rapid method for the determination of 5 JAK inhibitor compounds illegally added to the dietary supplements.Methods:The determination was performed by LC-MSMS,and the separation was achieved on a CAPCELL PAK C_(18)(3.0 mm×100 mm,3 μm)column in a gradient elution mode with 0.1% formic acid water and 0.1% formic acid acetonitrile as the mobile phase at a flow rate of 0.4 ml·min^(-1),the column temperature was 35℃,the mass spectrometry parameters were as follows:electrospray ionization(ESI),positive ion scan mode and a multiple reaction monitoring(MRM) mode were used to quantitatively determine the 5 JAK inhibitors,and the illegally added compounds were confirmed by comparing the molecular ion peak,product ion peak and retention time between the reference standards and the samples in different transitions.Results:The five JAK inhibitors were separated well,the method LODs were between 0.02 and 0.21 ng·ml^(-1),the LOQs were between 0.05 and 0.45 ng·ml^(-1),and the average recoveries were between 91.2% and 102.9%.Conclusion:The method is simple and accurate,and can be used for the determination of illegally added JAK inhibitors in dietary supplements.
作者
李慧玲
王嘉林
Li Huiling;Wang Jialin(Anyang Food and Drug Inspection and Testing Center,Henan Anyang 455000,China;Luoyang Institute for Food and Drug Control)
出处
《中国药师》
CAS
2022年第4期746-749,共4页
China Pharmacist
