LC-DAD-MS/MS法检测抗风湿中药制剂中非法添加的双氯芬酸盐  

Determination of Diclofenac Salt Illegally Mixed into Traditional Chinese Medicinal Preparation by LC-DAD-MS/MS

作　　者：许美娟[1] 邹建东[1] 卜擎燕[1] 熊宁宁[1] 许黎君[1] 谈恒山[2] 居文政[1] 

机构地区：[1]南京中医药大学附属医院临床药理试验室,南京210029 [2]南京军区总医院

出　　处：《中国药师》2010年第10期1396-1398,共3页China Pharmacist

基　　金：国家十一五研究课题(编号:2006BA104A21)

摘　　要：目的:采用液相色谱-二极管阵列-串联质谱检测法(LC-DAD-MS/MS)定性、定量检测某抗风湿中药中非法添加的双氯芬酸盐。方法:选用Agilent ZORBAX SB C_(18)(150 mm×4.6 mm,5μm)柱,以甲醇-20 mmol·L^(-1)乙酸铵溶液(60:40)为流动相,对非法制剂的提取液进行分析。通过与对照品的色谱保留时间、紫外吸收光谱及质谱碎裂行为的比较,对此类药进行定性鉴别和定量测定。结果:某抗风湿中药胶囊剂两个批次均检测到了西药双氯芬酸盐。结论:所用方法专属性强、灵敏度高、操作简便,可作为分析中药中非法添加双氯芬酸盐的参考方法。Objective： To establish a liquid chromatography coupled with diode array detector and tandem mass spectrometry method （LC-DAD-MS/MS） for qualitative and quantitative determination the illegally added ingredient diclofenac salts in Traditional Chinese Medicine （TCM）. Method： Agilent ZORBAX C 18 （150 mm × 4.6 mm ,5 μm）column was used with a mobile phase of methanol and 20 mmol· L^- 1 ammonium acetate solution （60： 40）. Diclofenac salt adulterated into TCM was identified according to the chromatographic behavior, the characteristic of ultraviolet absorption and mass spectral data by comparison with the reference substance. Result： Diclofenac salt was found in the tested TCM preparation and qualitatively determined. Conclusion： The method is selective, sensitive, simple, and can be used to detect diclofenac salt illegally added into TCM preparation.

关 键 词：液相色谱-二极管阵列-串联质谱法 中药制剂 双氯芬酸 

分 类 号：R917[医药卫生—药物分析学]