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目的:建立无需更换流动相而可用于中成药中非法添加化学成分现场快速筛查的HPLC-DAD法。方法:采用岛津Shim-pack VP-ODS色谱柱,使用2种等组成的流动相:Ⅰ为乙腈-0.02 mol.L-1甲酸铵缓冲液(pH3.8)(50∶50);Ⅱ为甲醇-0.01 mol.L-1乙酸铵(35∶65)。检测波长229 nm,参比波长550 nm,DAD波长扫描范围190~600 nm。测定时先将样品检出峰的保留时间与对照品比较,找出保留时间一致的疑似物;再将疑似物的光谱与相应的对照品比较。结果:建立的色谱条件可以分离消渴类中成药中常见的10种非法化学添加成分;循环使用流动相进样150次后,除基线稍有提高外,色谱峰分离度和理论塔板数均未明显变化;采用循环使用150次后的流动相成功筛查出未知样品中的非法添加物格列本脲,并得到了LC-MS的确认。结论:将流动相循环使用检测多个样本是可行的,适合现场采用车载或便携式HPLC仪进行快速药品筛查的需要;本文建立的色谱条件可以用于快速筛查消渴类中成药中的非法添加化学成分。
OBJECTIVE: To establish an HPLC-DAD method for rapidly screening unlawfully added chemical components in proprietary Chinese medicines without changing the mobile phase. Methods: Shimadzu Shim-pack VP-ODS column was used with two mobile phases: Ⅰ acetonitrile-0.02 mol·L-1 ammonium formate buffer (pH 3.8) (50:50), Ⅱ Methanol - 0.01 mol. L-1 ammonium acetate (35:65). The detection wavelength is 229 nm, the reference wavelength is 550 nm and the wavelength range of DAD is 190-600 nm. Determination of the first sample peak retention time compared with the control to find the same retention time of the suspected substance; then the suspect spectrum compared with the corresponding reference substance. Results: The chromatographic conditions established could separate 10 kinds of illegal chemical components commonly found in Chinese traditional medicines for diabetes. After the mobile phase was injected 150 times, the chromatographic peak resolution and theoretical plate number No significant changes were observed. The glyphosate, an illegal additive in unknown samples, was screened by mobile phase after 150 cycles, and LC-MS was confirmed. Conclusion: It is feasible to use mobile phase to test multiple samples, which is fit for on-the-spot or in-line HPLC instrument for rapid drug screening. The chromatographic conditions established in this paper can be used for rapid screening of illegal Chinese medicines Add chemical composition.