超高效液相色谱-串联质谱法测定食品中10种降尿酸类药物

Determination of 10 kinds of uric acid-lowering drugs in foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  降尿酸  食品  高尿酸血症  痛风  超高效液相色谱-串联质谱  非法添加

英文关键词:uric acid-lowering drugs  hyperuricemia  gout  ultra performance liquid chromatography-tandem mass spectrometry  illegal addition

中文摘要:

      目的 建立超高效液相色谱-串联质谱法定量测定食品中非法添加的降尿酸类物质的分析方法。方法 样品经甲醇、5%甲醇溶液为提取溶剂, 经超声提取, C18色谱柱分离, 以含0.1%甲酸水溶液和甲醇为流动相梯度洗脱, 采用质谱多反应监测(multiple reaction monitoring, MRM)方式, 外标法定量。结果 在溶剂曲线中, 别嘌醇、秋水仙碱、托匹司他、雷西那德、曲尼司特在20~400 ng/mL范围内线性相关系数均大于0.999, 利培酮、非诺贝特、非布司他、丙磺舒、苯溴马隆在2~40 ng/mL范围内线性相关系数均大于0.999, 在片剂(压片糖果)、液体饮料、固体饮料、花粉、泡腾片5种基质中测定3个水平加标回收率范围为81.62%~109.61%, 相对标准偏差(relative standard deviations, RSDs)为1.0%~8.6% (n=6)。结论 本方法准确度高、精密度好、重现性高, 仪器间适用性好, 可满足于测定食品中别嘌醇等10种降尿酸类化合物的定性定量分析。

英文摘要:

      Objective To establish a quantitative analysis method for determining illegally added uric acid-lowering substances in food by ultra performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with methanol and 5% methanol solution as the extraction solvent, and extracted by ultrasound, and then separated on a C18 column with a gradient elution of 0.1% form acid aqueous solution and methanol as the mobile phase. The detection was performed using multiple reaction monitoring (MRM) mode of mass spectrometry, and quantification was done by external standard method. Results In the solvent curve such as allopurinol, colchicine, topiroxostat, lesinurad and tranilast all showed linear correlation coefficients of r>0.999 in the range of 20–400 ng/mL, while risperidone, fenofibrate, febuxostat, probenecid and benzbromarone showed linear correlation coefficients of r>0.999 in the range of 2–40 ng/mL. The recovery rates ranged from 81.62% to 109.61% within 3 levels in 5 kinds of matrices such as tablets (compressed candy tablets), liquid beverage, powdered beverage, pollen and effervescent tablet and the relative standard deviations (RSDs) were 1.0% to 8.6% (n=6). Conclusion This method has high accuracy, good precision, high reproducibility and good applicability between instruments, and can meet the needs of qualitative and analysis of allopurinol and other 10 kinds of uric acid-lowering compounds in food.