亚3μm填料核壳技术结合UPLC法快速测定降血脂类中成药及保健食品中12种非法添加物

Rapid Determination of Twelve Lipid-lowing Illegal Additives in Traditional Chinese Medicine and Health Food by UPLC Coupled with Sub-3 μm Particle Fused-core Column

目的:建立亚3μm填料核壳技术结合UPLC法快速测定降血脂类中成药及保健食品中12种非法添加化学药物。方法:样品采用甲醇提取,经Agilent Poroshell 120 EC-C18色谱柱(4.6 mm×100 mm,2.7μm)分离,以20mmol·L^(-1)乙酸铵水溶液和甲醇为流动相梯度洗脱,流速1.0 ml·min^(-1),采用二极管阵列检测器检测,采集波长230 nm处的色谱图进行粗筛和定量,并通过与12种降脂药物对照品的光谱比对进行确证。结果:本方法可在19min内同时分离12种化学药物。12种化合物在0.10~50.00μg·ml^(-1)的线性范围内相关系数(R2)均大于0.999,检出限为5 mg·kg^(-1),平均加标回收率范围为73.2%~108.2%,RSD均低于6.9%。利用建立的高效液相色谱法检测了30批降血脂类中成药及保健品,其中2批检出含有洛伐他汀、去羟基洛伐他汀、洛伐他汀羟酸钠盐等化学成分。结论:本方法可用于降血脂类中成药及保健食品中12种非法添加化学药的高通量筛查和定量检测。

Objective: To rapid determine twelve lipid-lowing illegal additives in traditional Chinese medicine and health food by UHPLC coupled with sub-3μm particle fused-core column. Methods: The samples were extracted with methanol. An Agilent Poroshell120 EC-C18 column(4.6 mm×100 mm,2.7 μm) was applied with the mobile phase consisting of 20 mmol·L^(-1) ammonium acetate and methanol in a gradient elution mode at the flow rate of 1.0 ml·min^(-1). The illegally added chemical drugs were detected by a photodiode array detector and a chromatogram with detection wavelength of 230 nm was used for screening and quantification. The results were then confirmed by comparison with the spectra of 12 reference substances. Results: The twelve chemicals could be analyzed within 19 min simultaneously. The correlation coefficients(R2) were all above 0.999 over the concentration range of 0.10-50.00 μg·ml^(-1). The detection limit was 5 mg·kg^(-1). The average recoveries ranged from 73.2% to 108.2% with the RSDs all below 6.9%. Thirty batches of traditional Chinese medicine and health food were tested by the methods,and 2 batches were found to contain lovastatin,lovastatin hydroxy acid and dehydro-lovastatin. Conclusion: The method can be used for the determination of twelve drugs illegally added to lipid-lowing Chinese traditional medicine and health food.