用于保健食品中6种非法添加降脂类药物的快速筛查与定量分析
目的 建立超高效液相色谱-四极杆/飞行时间高分辨质谱法快速测定保健食品中烟酸、辛伐他汀、美伐他汀、洛伐他汀、去羟基洛伐他汀和洛伐他汀羟酸钠盐的方法。方法 采用Waters ACQUITY UPLC HSS T3色谱柱, 以0.1%甲酸(V:V)-甲醇为流动相梯度洗脱, 流速0.3 mL/min, 柱温35 ℃, 在电喷雾离子源、正离子模式下, 以多反应监测方式检测6种非法添加降脂类药物。结果 6种化合物标准品溶液浓度和检测响应的线性关系良好, 其相关系数r均大于0.998; 检出限在0.56~50.10 ng/mL, 定量限在1.67~100.20 ng/mL, 方法准确度、精密度、重复性均可满足要求。结论 该方法简单、准确、高效, 可用于保健食品中6种降脂类药物的快速筛查和定量测定。
Objective To establish a method for determination of nicotinic acid, simvastatin, mevastatin, lovastatin, dehydro lovastatin and lovastatin hydroxy acid sodium salt in health food by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry (UPLC/Q-TOF-HRMS). Methods A Waters ACQUITY UPLC HSS T3 chromatographic column was used with the mobile phase of 0.1% (V:V) formic acid aqueous solution-methanol for gradient elution, the flow rate was 0.3 mL/min, and the column temperature was 35 ℃. Electrospray ionization (ESI) source was applied and operated in positive mode, 6 lipid-lowering drugs illegally added in health food were detected by multiple reactions monitoring (MRM) mode. Results Six lipid-lowering drugs had good linear relationships, and the correlation coefficients were greater than 0.998. The limits of detection of 6 lipid-lowering drugs were 0.56-50.10 ng/mL, and the limits of quantitation were 1.67-100.20 ng/mL. Precision, accuracy and repeatability was all satisfied. Conclusion This method is simple, accurate and efficient, which is suitable for rapid screening and quantitative analysis of 6 illegally added drugs in lipid-lowering health foods.
标题：用于保健食品中6种非法添加降脂类药物的快速筛查与定量分析
英文标题：Rapid screening and quantitative analysis of 6 kinds of lipid-lowering drugs illegally added in health food by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry
作者：
王小兵 山东省食品药品检验研究院
李启艳 山东省食品药品检验研究院
冉金凤 山东省食品药品检验研究院
冷佳蔚 山东省食品药品检验研究院
中文关键词:超高效液相色谱-四极杆/飞行时间高分辨质谱法,非法添加,保健食品,降脂类药物,快速筛查,
英文关键词:ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry,illegally added,health food,lipid-lowering drugs,rapid screening,
发表日期：2019-01-09
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