超高效液相色谱-四极杆/飞行时间高分辨质谱测定保健食品及其原料中洛伐他汀及类似物的含量

Simultaneous determination of lovastatin and its analogues in health food and raw materials by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry

中文关键词:  超高效液相色谱-四极杆/飞行时间高分辨质谱  保健食品  保健食品原料  洛伐他汀  洛伐他汀类似物

英文关键词:ultra performance liquid chromatography tandem quadrupole/time of flight high resolution mass spectrometry  health food  health food raw materials  lovastatin  lovastatin analogues

中文摘要:

      目的 利用超高效液相色谱－四极杆/飞行时间高分辨质谱(ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry, UPLC-Q/TOF HRMS), 建立同时鉴别和定量测定保健食品及其原料中的洛伐他汀及其类似物的分析方法。方法 样品用Agilent Eclipse Plus C18(50 mm×2.1 mm, 1.8 μm)色谱柱分离, 以甲醇和0.1%甲酸溶液作为流动相进行梯度洗脱, 电喷雾正离子模式离子化, 全扫描模式检测。结果 当称样量为1 g时, 酸式洛伐他汀、洛伐他汀、美伐他汀、辛伐他汀、去羟基洛伐他汀和洛伐他汀羟酸钠盐的检出限分别为40、25、25、25、25和50 ng/g; 洛伐他汀、美伐他汀、辛伐他汀、去羟基洛伐他汀在25~200 μg/L范围、洛伐他汀羟酸钠盐在100~800 μg/L范围内线性关系良好(R≥0.99); 5种成分在保健食品及原料中均有较好的回收率和稳定性。结论 该方法简便、快速、灵敏、准确, 适合于保健食品及原料中的洛伐他汀及其类似物的鉴别和定量测定。

英文摘要:

      Objective To establish a method for simultaneous determination of lovastatin and its analogues in health food and raw materials by ultra performance liquid chromatography tandem quadrupole/time-of-flight high resolution mass spectrometry (UPLC-Q/TOF HRMS). Methods Samples were analyzed by Agilent eclipse plus C18 column (50 mm×2.1 mm, 1.8 μm) with methanol and 0.1% formic acid solution as mobile phase. The ionization mode was electrospray positive mode and the detection mode was full scan. Results When the sample weight was 1 g, limits of detection of lovastatin acid, lovastatin, mevastatin, simvastatin, dehydro lovastatin and lovastatin hydroxy acid sodium salt were 40, 25, 25, 25, 25 and 50 ng/g, respectively. The linear ranges of lovastatin, mevastatin, simvastatin and dehydro lovastatin were 25~200 μg/L, and lovastatin hydroxy acid sodium salt was 100~800 μg/L (R≥0.99). Five kinds of substances had good recoveries and stability in health food and raw materials. Conclusion The established method is simple, rapid, sensitive and accurate, which is suitable for the identification and quantitative determination of lovastatin and its analogues in health food and raw materials.