超高效液相色谱-高分辨质谱法检测保健食品中14种降血糖类药物

Determination of 14 antidiabetic drugs in health foods by ultra performance liquid chromatography-high resolution mass spectrometry

中文关键词:  降血糖类药物  超高效液相色谱-高分辨质谱法  保健食品

英文关键词:antidiabetic drugs  ultra performance liquid chromatography-high resolution mass spectrometry  health food

中文摘要:

      目的 建立超高效液相色谱-高分辨质谱法(ultra performance liquid chromatography-high resolution mass spectrometry)检测不同剂型保健食品中14种降血糖类药物的分析方法。方法 样品经甲醇-水(8:2, V:V) 提取液提取, C18吸附剂净化。经ZORBAX SB Aq C18(100 mm×2.1 mm, 3.0 m)色谱柱分离, 以0.1%甲酸(A)和0.1%甲酸-乙腈(B)作为流动相, 梯度洗脱。采用电喷雾电离, 正离子检测, 全扫描-数据依赖二级扫描模式(Full-MS/dd-MS2)进行筛查, 全扫描模式(Full-MS)进行定量。结果 14种降血糖类药物在一定浓度范围内具有良好的线性关系, 相关系数(r2)大于0.99。14种降血糖类药物在0.5、1.0和5.0 mg/kg添加水平的回收率为69.6%%~109.4%, 相对标准偏差小于10% (n=6), 方法定量限为1.0 mg/kg。结论 该方法快速、准确、灵敏, 适合测定不同剂型保健食品中14种降血糖类药物。

英文摘要:

      Objective To establish a method for determination of 14 antidiabetic drugs in health foods by ultra performance liquid chromatography-high resolution mass spectrometry. Methods Samples were extracted with methnol-H2O (8:2, V:V), and cleaned by C18 sorbent. The chromatographic separations were performed on an Agilent SB Aq C18 column (100 mm×2.1 mm, 3.0 m) with 0.1% formic acid solution and acetonitrile as mobile phase by gradient elution. The MS analysis was operated under the positive electrospray ionization mode. Data obtained under the Full Ms/dd-MS2 scan mode or Full MS mode was used for confirmation or quantitaton, respectively. Results The 14 kinds of antidiabetic drugs had a good linear relationship within a certain concentration range, and the correlation coefficient (r2) was greater than 0.99. The recoveries of 14 antidiabetic drugs at the supplemental levels of 0.5, 1.0 and 5.0 mg/kg were 69.6%%-109.4%, the relative standard deviations were less than 10% (n=6), and the limit of quantification of the method was 1.0 mg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting antidiabetic drugs in different dosage forms of health foods.