目的 建立一种高效液相色谱-串联质谱法测定保健食品中抗风湿类药物含量的分析方法.方法 样品经超声提取和稀释后利用ZORBAX Eclipse Plus RRHD C18(3.0×150 mm,1.8 μm)色谱柱分离,通过流动相0.1％甲酸-5 mmol/L乙酸铵水溶液(A)-甲醇(B)梯度洗脱,多反应监测模式(multiple reaction monitoring,MRM)测定,外标法定量.结果 28种化合物在线性范围内线性关系良好,决定系数(R2)均≥0.99,检出限(limits of detection,LOD)为0.18～4.05 ng/mL;定量限(limits of quantitation,LOQ)为0.29～11.85 ng/mL;平均回收率介于62.1％～116.4％;平均相对标准偏差为1.1％～13.3％.结论 该方法可用于保健食品中非法添加抗风湿类药物的定性定量分析.
Determination of 28 kinds of illegally added anti-rheumatic drugs in health food by high performance liquid chromatography tandem mass spectrometry method
Objective To develop a high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method for the determination of 28 anti-rheumatic drugs in health food.Methods After ultrasonic extraction and dilution,the separation was achieved on a ZORBAX Eclipse Plus RRHD C18(3.0×150 mm,1.8 μm)column in a gradient elution mode with water(0.1％formic acid-5 mmol/L ammonium acetate)(A)and methanol(B),positive ion scan mode and a multiple reaction monitoring(MRM)mode were used to quantitatively determine the illegally added compounds by external standard method.Results The linear relationship of 28 compounds was good in the linear range,with determination coefficients(R2)≥0.99,the limits of detection(LODs)were 0.18-4.05 ng/mL,the limits of quantitation(LOQs)were 0.29-11.85 ng/mL,the average recoveries were 62.1％-116.4％,and the mean relative standard deviation were 1.1％-13.3％.Conclusion This method can be used for qualitative and quantitative analysis of illegally added anti-rheumatic drugs in health food.
Anti-rheumaticIllegal additiveHigh performance liquid chromatography tandem mass spectrometry methodHealth foods
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