UPLC-PDA快速识别抗感冒类中成药及保健食品中15个化学物质

Rapid identification of 15 chemical components in anti-common cold Chinese traditional patent medicine and health foods by UPLC-PDA

目的:建立超高效液相色谱(UPLC)法快速识别及定量分析抗感冒类中成药及保健食品中15个化学物质。方法:样品以1%醋酸甲醇溶液超声提取,离心后取上清液,选用Waters HSS T3(2.1 mm×100 mm,1.8μm)色谱柱进行分离,乙腈-0.1%磷酸溶液梯度洗脱,流速0.3 m L·min^(-1),柱温40℃,检测波长210 nm,对15个抗感冒类化学物质进行定性、定量检测。结果:15个化合物质量浓度在4.860~110.2μg·m L^(-1)范围内线性良好,相关系数均大于0.9995,各类化合物的检测下限为0.09~0.11μg·m L^(-1),回收率为97.0%~108.6%,RSD为0.43%~2.1%。应用该方法对10批次样品进行检测,共有6批检出,其中2批中成药检出对乙酰氨基酚和马来酸氯苯那敏,4批保健食品检出对乙酰氨基酚、马来酸氯苯那敏、醋酸泼尼松、双氯芬酸钠、布洛芬。结论:本方法操作简便,分析时间短,精密度、稳定性、重复性好,能够达到快速识别抗感冒类中成药及保健食品中添加化学成分的目的。

Objective:To establish an UPLC method for rapid identification and quantitation of 15 chemical components in anti-common cold Chinese traditional patent medicine and health foods.Methods:The samples were extracted by ultrasonic machine with 1%acetic acid methanol solution.After centrifugation,the supernatant was injected and the separation was performed on a Waters HSS T3 column(100 mm×2.1 mm,1.8μm)and the column temperature was set at 40℃.The mobile phase was composed of acetonitrile and 0.1%phosphoric acid with gradient elution at a flow rate of 0.3 m L·min^(-1).The detection wavelength was set at 210 nm for qualification and quantification.Results:The linearity of all the 15 drugs ranged from 4.860μg·m L^(-1)to 110.2μg·m L^(-1)with the correlation coefficients of greater than 0.9995.The limits of detection were between 0.09 and 0.11μg·mL^(-1),and the recoveries were in the range of 97.0%to 108.6%,with the relative standard deviations of 0.43%to 2.1%.Using this method,6 batches of positive samples were detected in 10 batches of samples.Paracetamol and chlorphenamine maleate were identified in two batches of anti-common cold Chinese traditional patent medicine,paracetamol,chlorphenamine maleate,prednisone acetate,diclofenac sodium,ibuprofen were found in four batches of health foods.Conclusion:The established method is simple,rapid,accurate,stable and reproducible,and it can be applied to the screening,confirmation and quantitation of 15 illegally added drugs in anti-common cold traditional Chinese medicine and health foods.