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目的在等度洗脱条件下建立10种化学降糖成分的HPLC-DAD数据库,用于消渴类中成药中非法添加成分的现场快速筛查。方法采用Waters XTerra MSC18(4.6 mm×150 mm,5μm)色谱柱,使用2种流动相:流动相I为乙腈-0.02%磷酸(55 45),流动相II为乙腈-0.01%三氟乙酸(25 75),检测波长229 nm,参比波长550 nm,波长扫描范围为190~600 nm。首先采集对照品的保留时间和光谱图,建立数据库;然后将样品中检出峰的保留时间与数据库比较,初筛出可疑的化学成分;最后将样品中可疑色谱峰的DAD光谱图与数据库中相应对照品的DAD光谱图比较,快速筛查出非法添加的化学成分,并对检出的化学成分进行LC-MS验证。结果 10种化学降糖成分在上述2种等度洗脱条件下实现了完全分离;采用本试验建立的方法检测了市售12批不同的消渴类中成药,发现其中5批含有非法添加成分,并且有1批同时含有4种非法降糖成分添加剂,LC-MS验证结果准确。结论本法可以准确有效地快速分离10种化学降糖成分,为消渴类中成药的现场打假提供有力的技术支持。
Objective To establish a HPLC-DAD database of 10 chemical hypoglycemic ingredients under isocratic conditions for rapid screening of illegally added components in Chinese patent medicines for diabetes. Methods A Waters XTerra MSC18 (4.6 mm×150 mm, 5 μm) column was used with two mobile phases: mobile phase I was acetonitrile-0.02% phosphoric acid (55 45), and mobile phase II was acetonitrile-0.01% trifluoroacetic acid (25 75) The detection wavelength is 229 nm, the reference wavelength is 550 nm, and the wavelength scanning range is 190-600 nm. Firstly, the retention time and spectrogram of the reference substance were collected to establish a database; then the retention time of the detected peak was compared with the database, and the suspected chemical components were initially screened out; finally, the DAD spectra of suspected chromatographic peaks in the sample and the database were collected. Comparing the DAD spectra of the corresponding reference materials, the illegally added chemical components were quickly screened and LC-MS verification was performed on the chemical components detected. Results The 10 kinds of chemical hypoglycemic ingredients were completely separated under the above two isocratic elution conditions; 12 batches of different Diabetes class proprietary Chinese medicines were tested by the method established in this experiment, and 5 of them were found to contain illegally added ingredients. , And there are 1 batches of 4 kinds of illegal hypoglycemic ingredients additives, LC-MS verification results are accurate. Conclusion This method can quickly and accurately separate 10 kinds of chemical hypoglycemic ingredients and provide powerful technical support for the anti-counterfeiting of Chinese medicines for diabetes.