通过式固相萃取-高效液相色谱-串联质谱法测定固体饮料、液体饮料、硬胶囊、软胶囊及压片糖果中他莫昔芬含量

Determination of tamoxifen content in solid drinks, liquid drinks, hard capsule, soft capsule and table candy by high performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction

中文关键词:  他莫昔芬  高效液相色谱-串联质法  非法添加  

英文关键词:tamoxifen  high performance liquid chromatography-tandem mass spectrometry  illegal additives

中文摘要:

      目的 建立一种高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)检测固体饮料、液体饮料、硬胶囊、软胶囊、压片糖果样品中他莫昔芬含量的方法。方法 样品经0.1%甲酸-乙腈溶液的超声提取剂, 提取液经通过式固相萃取小柱对固体饮料、液体饮料、硬胶囊、软胶囊和压片糖果中的他莫昔芬进行净化后过膜上机检测。以Agilent Eclipse Plus RRHD C18色谱柱(100 mm×2.1 mm, 1.8 μm)进行分离, 电喷雾正子模式, 串联质谱进行检测, 外标法定量。结果 他莫昔芬质量浓度在1.0~100.0 ng/mL线性关系良好, 相关系数在0.999以上; 检出限为0.015 mg/kg, 定量限为0.05 mg/kg。结论 该方法灵敏度高, 稳定性好, 操作简单, 可满足固体饮料、液体饮料、硬胶囊、软胶囊、压片糖果中他莫昔芬检测的精密度和灵敏的度要求。

英文摘要:

      Objective To establish an method for the determination of tamoxifen in solid drinks, liquid drinks, hard capsules, soft capsules and table candy by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 0.1% formic acid acetonitrile solution as ultrasonic extractant, and the analytical solution was purified by pass-through solid-phase extraction to detect tamoxifen in solid drinks, liquid drinks, hard capsules, soft capsules and tablet candy. Agilent Eclipse Plus RRHD C18 column (100 mm×2.1 mm, 1.8 μm) was used for separation, electrospray negative ion mode, tandem mass spectrometry for detection, and external standard method for quantification. Results That concentration of tamoxien was good linear relationship within the range of 1.0–100.0 ng/mL, and the correlation coefficient was above 0.999; the limit of detection was 0.015 mg/kg; The limit of quantitation was 0.050 mg/kg. Conclusion The method has been verified by the method with high sensitivity, good stability and simple operation, which can meet the requirements of precision and sensitivity for the detection of tamoxifen in solid drinks, liquid drinks, hard capsules, soft capsules and tablet candy.