| Hyperlipidemia is a common disease in the elderly, but also a disease that seriously concerned and affects the quality of life of elderly. In recent years, with the aging of the population increased and the living standards rised year by year,and improved nutrition and the average life expectancy. The average age of onset of hyperlipidemia has shown a obviously decline, and its complications(such as coronary heart disease, atherosclerosis, hypertension, etc.) has become a huge challenge because of the rising morbidity of hyperlipidemia. Currently, the lipid-lowering drugs are widely used in clinic can be divided into five kinds: statins, fibrates, niacin, bile acid sequestrants and cholesterol absorption inhibitors. Which statin is the major drug of treatment of hypercholesterolemia, but the most common adverse reactions of these drugs are mild gastrointestinal reactions and headaches. Even, muscle toxicity may occur in combination with other lipid-lowering drugs. Chinese herbal drugs preparations is based on the theory of natural herbs and development drugs of Chinese medicine, which play an important role in the practice of long-term clinical care and treatment. Chinese herbal drugs preparations is consist of various compound preparation that is the main feature of it, which can be directly used for disease prevention and control and it is safe, effective, easy to take, and the dose can be controlled. Compared with conventional chemicals drugs, Chinese herbal drugs have more advantages, such as less toxic side effects, safety, fewer side effects and so on. Studies also confirmed that Chinese herbal drugs compound preparations could slow down or terminate the process of atherosclerosis except reducing blood fat effect; making great therapeutic effect by long-term use.As a result of lipid-lowering class of Chinese herbal drugs compound preparations have Complicated components, which brings great difficulties to develop quality standards and test methods. With the rapid development of market economy, the market competition is increasingly intense and there is a corresponding change in the production, sale and purchase of medicines. Which lead to Chinese herbal drugs compound preparations have a unstable quality. Controllability of the quality of medicines is a fundamental property, and is a basis of the safety and effectiveness of drugs. Quality standards are the important means of controlling the quality of medicines, and the concrete embodiment of the quality control. Therefore, in order to make widely and safely application of lipid-lowering class of Chinese herbal drugs compound preparations, quality control of its index components has become the main target of our study. Jiangzhiling tablets, Xuezhiling tablets, Juemingjiangzhi tablets and Jiangzhining granules were selected as the research subjects to study; High performance liquid chromatography was used to control the compound preparations quality, committed systematic methodology verification and determination and the fingerprints of Jiangzhining granules were analyzed. The method is highly specific, good precision and stability. The experiment results were accurate and reliable, which could supply effective accordance and scientific with control the quality of lipid-lowering class of Chinese herbal drugs compound preparations. Part one Simultaneous determination of four anthraquinones inJiangzhiling Tablets by RP-HPLCObjective:To develop a simultaneous analysis method for Aurantio-obtusifolin, Aloeemodin, Emodin and Physcion in Jiangzhiliing tablets by HPLC.Methods:The four constituents were separated on an Kromasil C18 column(250 mm×4.6 mm, 5 mm) using a mobile phase consisted of methanol-0.1% phosphoric acid in water at the detection wavelength of 286 nm.Results:The calibration curves of Aurantio-obtusifolin, Aloeemodin, Emodin and Physcion were separated from imputities well and its linear in ranges of 16.7-134, 11.1-89.1, 90.3-722 and 97.9-797 ng.The average recoveries were 98.7%, 98.5%, 98.5% and 102.0% with RSDs of 0.3%, 1.0%, 0.7% and 0.3%, respectively.Conclusion:The method is rapid, simple, accurate and with good reproducibility and can be used in quality control of Jiangzhiling tablets. Part two Simultaneous quantitive determination of five chemicalcompositions in Xuezhiling Tablets by RP-HPLCObjective:An RP-HPLC method was established for the determination of the stilbene glucoside, Aurantio-obtusifolin, Emodin, Chrysophanol and Physcion in Xuezhiling Tablets.Methods:The chromatographic separation was achieved on an Kromasil C18 column(250 mm×4.6 mm, 5 mm) with acetonitrile-0.1% phosphoric acid in water as mobile phases at the flow rate of 1.0 m L/min for gradient elution with the detection wavelength of 286 nm.Results:The calibration curves of stilbene glucoside,Aurantio-obtusifolin, Emodin, Chrysophanol and Physcion were linear in ranges of 2.04-20.4, 0.0836-0.836, 0.113-1.13, 0.0491-0.491 and 0.174-1.74 ug. The average recoveries were 96.5%, 97.2%, 97.9%, 96.9%, 99.2%;with RSDs of 0.57%, 1.1%, 1.2%, 0.71% and 0.95%, respectively.Conclusion:The method is accurate, credible, sensitive, and repeatable. It could be applied to the quality control of Xuezhiling Tablets. Part three Simultaneous Determinatian of Stilbene glucoside, Emodinand Physcion in Jueming Jiangzhi Tablets by RP-HPLCObjective:An liquid chromatography,(HPLC) method was established for the determination of the stilbene glucoside, Emodin and Physcion in Jueming Jiangzhi Tablets.Methods:HPLC system was carried out on an Kromasil C18 column(250 mm×4.6 mm, 5 mm) with acetonitrile-0.1% phosphoric acid in water as mobile phases. The column temperature was 30℃ and the flow rate of 1.0 m L/min. The nuciferine was detected at the wavelength of 288 nm.Results:Under the selected chromatographic conditions, stilbene glucoside, emodin and physcion were separated completely. Regression equation of stilbene glucoside was Y=1.27×102X+825(R=0.9992), showed a good linear relationship in the range of 1.39-9.71mg,the average recovery was 98.6%, and its RSD rates was 1.2%(n=6); Regression equation was Y = 3.39× 103 X + 1.06(R=1.0000), the liner in the range of emodin was 0.0677-0.474mg, the average recovery was 98.6%, and its RSD rates was 1.1%(n=6); Regression equation of Physcion was Y= 2.14 × 103X- 6.66(R=0.9999), its linear in range of 0.0740-0.518mg, the average recovery was 98.4%, and its RSD rates was 1.0%(n=6).Conclusion:The method is simple, accurate,sensitive, and repeatable. which can be used for determination of the content of the stilbene glucoside, Emodin and Physcion in Jueming Jiangzhi Tablets. It could be applied to the quality control of Jueming Jiangzhi Tablets. Part four Simultaneous quantitive determination of five chemicalcompositions in Jiangzhining granules from differentmanufacturers by RP-HPLCObjective:An liquid chromatography,(HPLC) method was established for the determination of the stilbene glucoside, Aurantio-obtusifolin, Emodin, Chrysophanol and Physcion in Jiangzhining.Methods:HPLC system was carried out on an Diamonsil C18 column(250 mm×4.6 mm, 5 mm) with acetonitrile-0.1% phosphoric acid in water as mobile phases. The flow rate of 1.0 m L/min and the column temperature was 30℃. The nuciferine was detected at the wavelength of 286 nm.Results:Under the selected chromatographic conditions, stilbene glucoside, Aurantio-obtusifolin, Emodin, Chrysophanol and Physcion were separated completely. Regression equation of stilbene glucoside was Y=23.6X+12.2(R=0.9991), showed a good linear relationship in the range of 0.45-3.15mg,the average recovery was 96.2%, and its RSD rates was 0.57%(n=6); Regression equation was Y = 1.24×102X-0.0984(R=0.9998), the liner in the range of Aurantio-obtusifolin was 0.0500-0.351mg, the average recovery was 96.8%, and its RSD rates was 0.85%(n=6); Regression equation of Emodin was Y = 1.01×102X-0.0674(R=0.9998), its linear in range of 0.0226-0.158mg, the average recovery was 98.2%, and its RSD rates was 0.81%(n=6). Regression equation was Y= 46.6X-0.0501(R=0.9997), the liner in the range of Chrysophanol was 0.0246-0.176mg, the average recovery was 98.0%, and its RSD rates was 1.1%(n=6); Regression equation of Physcion was Y= 55.4X- 0.0191(R=0.9997), its linear in range of 0.00752-0.0526mg, the average recovery was 97.2%, and its RSD rates was 1.2%(n=6)Conclusion:The method is simple, accurate,sensitive, and repeatable. which can be used for determination of the content of the stilbene glucoside, Aurantio-obtusifolin, Emodin, Chrysophanol and Physcion in Jiangzhining. It could be applied to the quality control of Jiangzhining. Part five RP-HPLC fingerprint of Jiangzhining granulesObjective:To develop a analysis method for the fingerprinting of Jiangzhining granules by RP-HPLC. Provide a reference for the production and the quality control of product process of Chinese herbal drugs compound preparations.Method:(1)Extraction:comparing different extraction solvent, extraction time and extraction method to ensure the maximum extraction rate.(2) Optimization of the chromatographic conditions: in order to ensure it compliance with the requirements of fingerprints, the systems and ratio of mobile phase、column temperature and detection wavelength were tested to determine the mobile phase chromatographic.(3) The test of precision: The systems precision was evaluated by analyzing five repeated injection of the same sample solution. The retention time and peak area were be recorded.(4)The test of stability: the test of stability was tested by determining the same sample solution stored at room temperature at different time of 0, 2, 4, 8, 12 h. The retention times and the peak areas of the major chemical components were analyzed for evaluation of the stability.(5)The test of reproducibility: reproducibility was assessed by analyzing five replications prepared from the sample within a day. The retention time and peak area were be analyzed.(6) The established method was used for establishment of fingerprints of Jiangzhining granules at ten different production batches,and the analysis results of similarities of HPLC fingerprints of Jiangzhining granules can be used to quality evaluation of Jiangzhining granules at different production batches.Results:(1)Extraction: The best extraction program is 75% methanol ultrasonic extraction in 45 min.(2) Optimization of the chromatographic conditions: The chromatographic separation was achieved on an Diamonsil C18 column(250 mm×4.6 mm, 5 mm) with acetonitrile(A)-0.1% phosphoric acid(B) in water as mobile phases at the flow rate of 1.0 m L/min for gradient elution with the detection wavelength of 286 nm.The gradient elution program is A:B(0~10min, 35:65; 10~60min, 35:65~10:90; 60~70min, 90 : 10),Pre-equilibrated time is 10 min. The analysis time is 70 minutes and the column temperature was 30℃.(3) The test of precision: the RSD of the relative retention times and the relative peak areas were between 0.87%~1.07% and between 0.84%~2.1%, respectively. And the precision of sample was good.(4) The test of stability: the RSD of retention times and the peak areas of the major peaks for the tests of sample were between0.76%~0.93% and between 0.87%~2.4%, respectively. The sample solution was stable within 12 hours.(5) The test of reproducibility: the RSD of retention times and peak areas of major peaks for the tests of sample were between 0.52%~0.62% and2.5%~2.9%.(6):The quality of different batches of Jiangzhining granules can be evaluated by similarity evaluation system, and Through this system, the fingerprinting of 10 different batches of particles Jiangzhining granules and 26 common peaks were measured.Conclusion:The method of HPLC fingerprint of Jiangzhining granules is feasible, and this method is stable, accurate, and has a good reproducible. Similarity evaluation system can effectively reflect and control the quality of different batches of Jiangzhining granules. |
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