超高效液相色谱串联质谱法检测16种中药乳膏制剂中抗真菌药  

Detection of Antifungal Drugs in 16 Traditional Chinese Medicine Cream Preparations by UPLC-MS/MS

作　　者：杨晓 薛文静 焦洁 YANG Xiao;XUE Wenjing;JIAO Jie(Qingdao Exchange for Government Services and Public Resources,Qingdao,Shandong,China 266071;Qingdao Institute for Food and Drug Control·NMPA Key Laboratory of Quality Research and Evaluation of Marine Traditional Chinese Medicine,Qingdao,Shandong,China 266071;Beijing Institute of Technology,Beijing,China 100081)

机构地区：[1]山东省青岛市政务服务和公共资源交易中心,山东青岛266071 [2]山东省青岛市食品药品检验研究院·国家药品监督管理局海洋中药质量研究与评价重点实验室,山东青岛266071 [3]北京理工大学,北京100081

出　　处：《中国药业》2025年第4期84-87,共4页China Pharmaceuticals

摘　　要：目的建立检测中药外用制剂中抗真菌药物的超高效液相色谱串联质谱(UPLC-MS/MS)法。方法以山东省疾病预防控制中心提供的16种中药乳膏制剂为检测对象。色谱柱为Agilent Poroshell SB-C18柱(100 mm×2.1 mm,2.7μm),流动相为0.1%甲酸水溶液-乙腈(含0.1%甲酸水溶液),梯度洗脱,流速为0.3 mL/min,柱温为30℃,进样量为2μL;电喷雾离子源,正离子、多反应监测模式,离子源温度为250℃,毛细管电压为3.5 k V,脱溶剂气温度为325℃。结果灰黄霉素、酮康唑、克霉唑、硝酸益康唑、硝酸咪康唑、氟康唑、联苯苄唑、氟胞嘧啶、盐酸萘替芬质量浓度分别在1~20 ng/mL、10~200 ng/mL、0.5~10 ng/mL、0.5~10 ng/mL、0.5~10 ng/mL、1~20 ng/mL、1~20 ng/mL、5~100 ng/mL、0.5~10 ng/mL范围内与峰面积线性关系良好(r≥0.995,n=6);精密度、稳定性、重复性试验结果的RSD均小于5.0%;平均加样回收率为83.14%~102.01%,RSD为1.60%~3.64%(n=9)。16种中药乳膏制剂均未检出上述9种抗真菌药物。结论所建立的方法操作简便、可靠、结果准确,可用于快速、有效地检测中药外用制剂中抗真菌药物的非法添加。Objective To establish an ultra-high-performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for detecting antifungal drugs in external preparations of traditional Chinese medicine(TCM).Methods Sixteen types of TCM cream preparations provided by the Shandong Center for Disease Control and Prevention were used as the testing objects.The chromatographic column was an Agilent Poroshell SB-C18 column(100 mm×2.1 mm,2.7µm),the mobile phase was 0.1%formic acid aqueous solution-acetonitrile(containing 0.1%formic acid aqueous solution)with gradient elution,the flow rate was 0.3 mL/min,the column temperature was 30℃,and the injection volume was 2µL.Electrospray ionization was adopted with positive ion,multi-reaction monitoring mode,the ion source temperature was 250℃,the capillary voltage was 3.5 kV,the desolvation gas temperature was 325℃.Results The linear ranges of griseofulvin,ketoconazole,clotrimazole,econazole nitrate,miconazole nitrate,fluconazole,bifonazole,flucytosine,and naftifine hydrochloride were in the range of 1-20 ng/mL,10-200 ng/mL,0.5-10 ng/mL,0.5-10 ng/mL,0.5-10 ng/mL,1-20 ng/mL,1-20 ng/mL,5-100 ng/mL,0.5-10 ng/mL,respectively(r≥0.995,n=6).The RSDs of precision,stability and repeatability tests were all lower than 5.0%.The average recovery rates were in the range of 83.14%to 102.01%with RSDs in the range of 1.60%to 3.64%(n=9).None of the above nine antifungal drug was detected in the 16 TCM cream preparations.Conclusion The established method is easy,reliable and accurate,which can be used for the rapid and effective detection of illegal addition of antifungal drugs in TCM external preparations.

关 键 词：非法添加 超高效液相色谱串联质谱法 抗真菌药物 中药外用制剂 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]