HPLC-DAD-MS联用法检测中药降糖制剂及胶囊壳中非法添加罗格列酮的研究

HPLC-DAD-MS detection of rosiglitazone mixed illegally into traditional Chinese medicinal antidiabetic preparation and shell of capsules of traditional Chinese medicinal antidiabetic preparation

目的:建立检测中药降糖制剂及胶囊壳中非法添加的罗格列酮的专属性方法。方法:采用液相色谱-质谱联用法,样品以 Agilent TC-C_(18)(250 mm×4.6 mm,5 μm)色谱柱进行分离,以甲醇-0.1%甲酸水溶液(30:70)为流动相,流速为1.0 mL·min^(-1),检测波长范围为200～400 nm,分流比为4:1。采用电喷雾离子化正离子检测模式(ESI^+),m/z 范围为100～800amu,毛细管电压为+3.2 kV,脱溶剂气(N_2)为350 L·h^(-1),锥孔反吹气为50 L·h^(-1),锥孔电压为45 V,脱溶剂温度为150℃,源温度为105℃,检测方式为全扫描质谱。通过液相色谱保留时间、紫外光谱图、相对分子质量及源内 CID(碰撞诱导裂解)碎片离子等信息,对中药降糖制剂及胶囊壳的提取液进行液相色普-质谱分析。通过与罗格列酮的色谱及质谱行为相比较,对中药降糖制剂及胶囊壳中非法添加的罗格列酮进行检测。结果:在市售某中药降糖制剂或胶囊壳中检测到罗格列酮。结论:该方法选择性强,灵敏度高,可用于非法添加化学降糖药罗格列酮的药品快速检测方法的研究。

Objective： To develop a specific method for detection of rosiglitazone added into traditional Chinese medicinal antidiabetic preparation and capsule shell. Methods： The liquid chromatography - mass spectrometry method was used. The HPLC separation was performed on an Agilent TC - C18 （250 mm × 4. 6 mm, 5 μm） column, using methanol-water（0. 1% formic acid）（30： 70）as mobile phase,with a flow rate of 1 mL · min^-1 ,the sample was detected at the range of 200 -400 nm, split ratio was 4： 1. And ESI ＋ was employed, the sample was analyzed in the positive -ion mode. The range of full scan was m/z 100 -800 amu, capillary voltage was ＋ 3.2 kV, desolvation gas （N2）flow was 350 L · h^-1 ,cone gas flow was 50 L · h^-1 ,the cone voltage was 45 V,desolvation temperature was 150 ℃ ,source temperature was 105 ℃. The retention time,the UV spectrum,relative molecular mass,CID fragment ion of the analytes was used to detect rosiglitazone in traditional Chinese medicinal antidiabetic preparation and capsule shell After separated by HPLC - DAD - MS ,the extraction of above samples was analyzed. The compounds illegally added into samples were detected according to the retention time, the UV spectrum,relative molecular mass, CID fragment ion of the analytes by comparison with rosiglitazone. Results： Rosiglitazone was found in traditional Chinese medicinal antidiabetic preparation and capsule shell of traditional Chinese medicinal antidiabetic preparation. Condusion：The method is selective,sensitive,and can be used to tacho-screen the illegal traditional Chinese medicinal antidiabetic preparations.