| ObjectiveZhengtian Pills (ZTP), an chinese patent medicine, is comprised of fifteen medicinal herbs including Spatholobi Caulis, Radix Angelicae sinensis, Ligusticum chuanxiong Hort, Herba asari. It has effect to neuro headache, tension headache, headache of Spinal disease cause, premenstrual headache, and is widely used for migraine in China. Though Spatholobi Caulis is indispensable ingredients of ZTP prescription, but the qulity is difficult to control in the current quality standard for its inferior products and adulterants.In this study, quality standards of Spatholobi Caulis and ZTP were studied with fast performance liquid chromatography,GC-MS and NIR technology, which provide a foundation for Spatholobi Caulis and ZTP’s quality control.Methods2.1Quality study of the crude drugs of Spatholobi CaulisThe water content and total ash were checked by the relevant provisions in Chinese Pharmacopeia2010. The microbial limit, heavy metal residues and pesticide residues were checked by "preparation and export of medicinal plants and green industry standard", which was promulgated by the Ministry of Commerce. And TLC method was adopted to identify formononetin of Spatholobi Caulis. NIR technology was used to evaluate the quality of the Spatholobi Caulis. The determination employed fast liquid chromatography to determine the contents of3marker compounds(protocatechuic acid, catechin and epicatechin) in18samples of Spatholobi Caulis, which were collected from different areas and markets. Specific chromatogram was used to analyze samples from crude drugs of Spatholobi Caulis. 2.2Quality study of Zheng Tian Pill(ZTP)The water, filling variation, weight variation of ZTP are checked by the relevant provisions of Pills in Chinese Pharmacopoeia2010. The determination employed fast liquid chromatography to determine the contents of3marker compounds (ferulic acid, protocatechuic acid, ligustilide) in13samples. The volatile components of ZTP were studied by gas chromatography mass spectrometry (GC-MS). Specific chromatogram was used to analyze samples from ZTP. Results3.1Quality study of the crude drugs of Spatholobi CaulisThe18batches of Spatholobi Caulis are met the Chinese Pharmacopoeia2010requirements in water and total ash. The TLC spots showed the same colors to the reference substances in the corresponding position. The microbial limit, heavy metals and pesticide residues determination Determination items of Spatholobi Caulis were all up to the standards.A NIR qualitative model was established that can distinguish the samples of Spatholobi Caulis from different sources.The UHPLC-DAD analysis methods were established to determine3components, which showed good linearity(r>0.999)in the range of the test concentration, and the average recoveries were98.58%-101.00%(RSD≤1.41). The content of protocatechuic acid is between0.0281-0.1567mg/g, catechin is between0.2898-0.7843mg/g, and epicatechin is between0.4691-1.9966mg/g,The HPLC-DAD analysis methods were established to determine formononetin. Its content is between0.0048-0.1887mg/g. The linear range of the formononetin determination was0.0014-3.576μg (r=0.9998), and the average recoverie (n=6) was101.77%(RSD=0.63%). The Specific chromatogram of HPLC-DAD were built up. The chromatogram of DAD has thirteen common peaks. And formononetin was used as reference compound. Meanwhile, the relative retention times of characteristic peaks were confired. The RSD of relative retention time of samples were less than or equal to0.1%.3.2Quality study of Zheng Tian Pill (ZTP)The13batches of ZTP are met the Chinese Pharmacopoeia2010requirements in water and weight variation. And the water content were in the range of2.9%-7.0%. The TLC spots showed the same colors to the reference substances in the corresponding position. And the negative control showed no interference. The UHPLC-DAD analysis methods were established to determine3components, which showed good linearity(r>0.999)in the range of the test concentration. The average recoveries were100.68%-102.69%. The content of protocatechuic acid is between0.0061-0.0173mg/g, ferulic acid is between0.0781-0.1159mg/g, and ligustilide is between0.0796-0.3887mg/g. The paeoniflorin of ZTP are met the Chinese Pharmacopoeia2010requirements. The Specific chromatogram of UHPLC-DAD were built up, which has nine common peaks, and the peak of ferulic acid, protocatechuic acid, ligustilide were used as reference compounds. Meanwhile, the relative retention time of characteristic peaks were confirmed. The RSD of relative retention time of samples were less than or equal to0.1%.21compounds in the extraction of ethyl acetate by ultrasonic method were identified by GC-MS., The contents of the main components of ZTP were determined by using the normalization method, include oleic acid, ligustilide,3,5-dimethoxybenzene,2-Methoxy-4-vinylphenol and methyl eugenol. Conclusions4.1Quality study of the crude drugs of Spatholobi CaulisA rapid liquid chromatography method was established for simultaneous determination of protocatechuic acid, epicatechin and catechin, which was simple and fast for the quality control of Spatholobi Caulis. The methods for determination of formononetin and specific chromatogram in Spatholobi Caulis were built up to control its quality. Qualitative model for Spatholobi Caulis detection by near infrared spectroscopy can help quickly identify Spatholobi Caulis from different sources.4.2Quality study of Zheng Tian Pill(ZTP)In this study, TLC, fast liquid chromatography, GC-MS chromatography, specific chromatogram techniques were used to improve quality control standards of ZTP. The results showed that the quality standard of ZTP is stable, specific, can be used as the evaluation method of the products... |
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