超高效液相色谱法同时测定降尿酸类保健食品中18种非法添加化学成分

Simultaneous determination of 18 kinds of illegally added chemical components in uric-acid-lowering health food by ultra performance liquid chromatography

中文关键词:  降尿酸  保健食品  非法添加  超高效液相色谱

英文关键词:uric-acid-lowering  health food  illegally addition  ultra performance liquid chromatography

中文摘要:

      目的 建立超高效液相色谱法同时测定降尿酸类保健食品中的18种非法添加化学成分的检测方法。方法 样品采用甲醇(含0.1%甲酸)超声提取, 经Phenomenex Luna ?Omega C18色谱柱 (2.1 mm×100 mm, 1.6 μm) 色谱柱分离, 以甲醇(A)-乙腈(B)-0.2%甲酸水溶液(C)为流动相进行梯度洗脱, 经过二极管阵列检测器检测。结果 该方法有效区分了水杨酸和阿司匹林, 并且18种降尿酸药物线性关系良好, 相关系数均大于等于0.9995; 检出限为2.0~112.8 mg/kg, 平均回收率为98.5%~110.6%, 相对标准偏差为0.2%~4.4%。应用该方法对35批样品进行筛查, 共有4批检出, 其中2批检测出双氯芬酸, 1批检测出吡罗昔康, 1批检测出醋酸泼尼松。结论 该方法操作简便, 具有良好的选择性、灵敏度及准确度, 能够用于降尿酸类保健食品中非法添加药物的测定。

英文摘要:

      Objective To established a method for the simultaneous determination of 18 kinds of illegally added chemical components in uric-acid-lowering health food by ultra performance liquid chromatography. Methods The samples were extracted by methanol (with 0.1% formic acid) ultrasonic extraction, the separation was executed on an Phenomenex Luna ?Omega C18 column (2.1 mm×100 mm, 1.6 μm), using methanol (A)-acetonitrile (B)-0.2% formic acid aqueous solution (C) as the mobile phase for gradient elution, and detected by diode array detector. Results This method effectively distinguishes between salicylic acid and aspirin and the results showed that the 18 kinds of uric-acid-lowering components had good linearity in the linear range with the correlation coefficients greater than or equal to 0.9995; the limits of detection ranged from 2.0–112.8 mg/kg, the average recoveries ranged from 98.5%–110.6%, and the relative standard deviations ranged from 0.2%–4.4%. The method was applied to screen 35 batches of samples, 4 batches of unlabeled components were detected, 2 batch detected diclofenac, 1 batch detected piroxicam and 1 batch detected prednisone acetate. Conclusion The method is easy to operate, has good selectivity, sensitivity and accuracy, and can be used for the determi nation of illegally added drugs of uric-acid-lowering components in health food.