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,1.8 μm） 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 mL·min-1. The detection wavelength was set at 210 nm for qualification and quantification. Results： The linearity of all the 15 drugs ranged from 4.860 μg·mL-1 to 110.2 μg·mL-1 with the correlation coefficients of greater than 0.999 5. The limits of detection were between 0.09 and 0.11 μg·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.
[1] 姜建国, 张西如, 张轶华, 等.LC-MS/MS 多反应监测快速识别抗感冒药中15个有效成分[J].药学学报, 2013, 48( 1):94
JIANG JG, ZHANG XR, ZHANG YH, et al.Rapid identification 15 effective components of anti commoncold medicine with MRM by LC-MS/MS[J].Acta Pharm Sin, 2013, 48( 1):94
[2] 符江, 荆文光, 章军, 等.中药中非法添加问题研究现状与分析[J].中草药, 2014, 45(3):437
FU J, JING WG, ZHANG J, et al.Research status and analysis of illegal addition in Chinese materia medica preparations[J].Chin Tradit Herb Drugs, 2014, 45(3):437
[3] 陈东洋, 张昊, 冯家力, 等.保健食品中违禁药物检验技术研究进展[J].色谱, 2020, 38( 8):880
CHEN DY, ZHANG H, FENG JL, et al.Advances in technologies for determination of illegal drugs in health food[J].Chin J Chromatogr, 2020, 38(8):880
[4] 谢志洁. 健康产品中非法添加化学成分快速筛查方法理论与实践[M].广州:华南理工大学出版社, 2011:51
XIE ZJ.Theories and Practices of Rapid Screening Technologies for Adulteration in Health Products[M].Guangzhou:South China University of Technology Press, 2011:51
[5] 施亚琴, 姚静, 张启明, 等.薄层色谱法快速筛查降血糖中成药及保健食品中添加磺酰脲类化学降糖药[J].药物分析杂志, 2007, 27(1):36
SHI YQ, YAO J, ZHANG QM, et al.TLC method for screening sulphonylureas inantidiabetics Chinese traditional patent medicines and health supplementary foods[J].Chin J Pharm Anal, 2007, 27(1):36
[6] 彭梦侠, 陈梓云, 姚婉清, 等.衰减全反射技术-红外光谱建模快筛中成药“骨节灵”中的丙酸类解热镇痛药[J].化学世界, 2017, 58(11):659
PENG MX, CHEN ZY, YAO WQ, et al.Rapid screening of propionic acid antipyretic analgesics in Chinese medicine “Gujieling”[J].Chem World, 2017, 58(11):659
[7] 宋占军, 董方霆, 魏开华, 等.应用FTIR 分析技术快速鉴定中药伟哥中的西地那非[J].解放军药学学报, 2003, 19(5):357
SONG ZJ, DONG FT, WEI KH, et al.Identification of sildenafil in the patent Chinese medicine-traditional Chinese viagra by FTIR[J].Pharm J Chin PLA, 2003, 19(5):357
[8] 邓鸣, 朱斌, 尹利辉.中成药及保健食品中非法添加调血脂类药物的HPLC 快速检测方法研究[J].药物分析杂志, 2016, 36(9):1639
DENG M, ZHU B, YIN LH.Rapid HPLC testing method for lipidregulating drugs illegally added in traditional Chinese medicines and health food[J].Chin J Pharm Anal, 2016, 36(9):1639
[9] 王豆, 杨欣, 程怡凡, 等.高效液相色谱法同时鉴定保健胶囊食品中非法添加的9 种降糖药成分[J].药物分析杂志, 2013, 33(8):1377
WANG D, YANG X, CHENG YF, et al.Identification of ninecomponents of antidiabetic medicine to health food capsules by HPLC[J].Chin J Pharm Anal, 2013, 33(8):1377
[10] 钱叶飞, 贾昌平, 鲁辉, 等.UPLC-MS/MS 法快速检测中成药及保健食品中非法添加38 种糖皮质激素[J].中国实验方剂学杂志, 2016, 22(10):60
QIAN YF, JIA CP, LU H, et al.Rapid determination of 38glucocorticoids illegally added into Chinese patent medicines and dietary supplements by UPLC-MS-MS[J].Chin J Exp Tradit Med Form, 2016, 22(10):60
[11] SHI F, GUO C, GONG L, et al.Application of a high resolutionbenchtop quadrupole-orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietarysupplements[J].J Chromatogr A, 2014, 1344(6):91
[12] LI H, AI LF, FAN SF, et al.Rapid determination of 18 glucocorticoids in serum using reusable on-line SPE polymeric monolithiccolumn coupled with LC-quadrupole/orbitrap highresolution masss pectrometer[J].J Chromatogr B, 2017, 1065(10):79
[13] 黄柳倩, 寿林均, 胡磊, 等.HPLC-MS/MS 法同时测定三高(高血糖、高血脂、高血压)人群用保健食品中添加的45 个化学药物[J].药物分析杂志, 2019, 39(3):484
HUANG LQ, SHOU LJ, HU L, et al.Simultaneous determination of 45 addition chemical drugs in hyperglycemic, hyperlipidemic and hypertensive people’s health foods by HPLC-MS/MS[J].Chin J Pharm Anal, 2019, 39(3):484
[14] 王小兵, 李启艳, 冉金凤, 等.超高效液相色谱-四极杆/ 飞行时间高分辨质谱法用于保健食品中 6 种非法添加降脂类药物的快速筛查与定量分析[J].食品安全质量检测学报, 2019, 10(5):1214
WANG XB, LI QY, RAN JF, et al.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[J].J Food Saf Qual, 2019, 10(5):1214
[15] 赵琪, 钱叶飞, 贾昌平, 等.UPLC-DAD 快速筛查抗风湿类保健食品及中成药中非法添加的19 个化学物质[J].药物分析杂志, 2019, 39(12):2171
ZHAO Q, QIAN YF, JIA CP, et al.Rapid determination of illegally added chemical drugs in anti-rheumatic Chinese traditional patent medicine and health foods by UPLC-DAD[J].Chin J Pharm Anal, 2019, 39(12):2171
