超高效液相色谱-四极杆飞行时间质谱测定抗风湿类中药非法添加的化学药物成分  

Determination of Chemical Components Illegally Mixed in Antirheumatic Traditional Chinese Medicine by Ultra-Performance Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry

作　　者：黄卫平[1] 李琴[2] 唐靓[3] 刘放[2] 

机构地区：[1]浙江医学高等专科学校,浙江杭州310053 [2]浙江省医学科学院药物研究所,浙江杭州310013 [3]浙江省医学科学院保健食品研究所,浙江杭州310013

出　　处：《中华中医药学刊》2014年第11期2707-2714,共8页Chinese Archives of Traditional Chinese Medicine

基　　金：浙江省公益性技术应用研究计划项目(2012C037045)

摘　　要：目的:建立快速、准确、高灵敏度的测定抗风湿类中药制剂中非法添加醋酸泼尼松、萘普生、醋酸地塞米松、双氯芬酸钠、吲哚美辛和布洛芬分析方法。方法:采用Waters ACQUITY BEH C18色谱柱(2.1 mm×50mm,1.7μm),以甲醇溶液为流动相A,0.1%醋酸的水溶液为流动相B,梯度洗脱。流速0.4 mL(min-1,Waters液相色谱-四级杆/飞行时间质谱,电喷雾离子源(ESI),毛细管电压为-2500 V,检测方式为负离子模式,一级、二级同时扫描。通过比较样品峰与对照品峰的保留时间、一级质谱和二级质谱碎片离子,确定样品中是否掺杂化学抗风湿药物。结果:建立的超高效液相色谱-串联质谱方法检测上述化学药物成分不受药物辅料干扰,各色谱峰分离良好,17批受试制剂中未检测到掺有上述药物。结论:此方法灵敏准确,可作为抗风湿类中药制剂中非法添加醋酸泼尼松、萘普生、醋酸地塞米松、双氯芬酸钠、吲哚美辛和布洛芬的有效检测方法。Objective ： To establish a quick, accurate, sensitive method for analysis of prednisone acetate, naproxen, dexamethasone acetate, diclofenac sodium, indometacin and ibuprofen illegally mixed in Ant rheumatic traditional Chinese medicine （TCM）. Method： The chromatographic conditions included Acuity BEH C19 analysis column （ 2. 1 mm× 50 mm, 1.7 μm ） , mobile phase of methanol （ A ） and water （0.1% acetic acid ） （ B ） with gradient elution, flow rate of was 0.4 mL（ min -1. The water liquid chromatography- quadrupole time - of - fight mass spectrometer （ LC - Q - TOF/ MS） was adopted with electrospray ion sourse （ESI）. the The Capillary vohage was - 2500 V. The detection mode ： simultaneous first and second level scanning with negative modes. The chemicals detected in samples were identified by comparison of sample peaks with the retention time, mass spectra and the product ions with those of refereneereference substances. Result ： The developpeddeveloped UPLC - QTOF/MS method was interfered not affected by the adjuvantsadjutants.. The detected peaks detected could be separated from each other. Seventeen different health - care plasters were identified, they They were not found illegally mixed. Conclusion：The method is sensitive and accurate, and can be used to detect the prednisone acetate, naproxen, diclofenac sodium, diclofenac sodium, indometacin and ibuprofen illegally mixed in ant anti -rheumatic traditional Chinese medicine.

关 键 词：超高效液相色谱 四极杆-飞行时间质谱 抗风湿类中药制剂 醋酸泼尼松 萘普生 醋酸地塞米松 双氯芬酸钠 吲哚美辛 布洛芬 

分 类 号：R284[医药卫生—中药学]