| Developed by a hospital, SGR oral is beneficial for blood and blood circulation. Clinically, it is widely used for the treatment of blood deficiency,palpitations caused by stasis, sweating, lochia and puerpera with the above symptom. Its prescription includes 12 pieces of herbal medicine like Astragalus, Rehmannia. In order to better control its quality, TLC of root of herbaceous peony, Angelica and Baizhu and component determination of Astragalus, root of herbaceous peony and Ferulic acid have been done. These measures not only raise the standard but also effectively control the quality of the medicine which further ensure safety and effectiveness of the medicine.Conduct a quality control study on SGR particles: apply TLC on root of herbaceous peony, angelica, Baizhu and Huangqi. Apply HPLC to determine the contents of Astragalus, root of herbaceous peony and ferulic acid. Negative control, stability test and recovery test have been conducted to prove the effectiveness and feasibility of the method.The first part TLC of SGR particlesObjective: To control the quality of SGR particles. Establish TLC of Baizhu, Angelica, Huangqi and root of herbaceous peony to determine their roles in the particle.Method:1 Development of sample solution,2 Contrastive medicine3 Selection and optimization of eluent,4 Coloring or fluorescent view.Result:1 Adopt TLC results of main components like as Baizhu, Angelica,Huangqi, root of herbaceous peony as quality control standards. Use Baizhu,Angelica and Chuanxiong as control herbal medicine and paeoniflorin as content control.2 Conduct a study on optimized TLC. Contrastive medicines show the same color or fluorescent spot at the same position with no negative control.Conclusion:The method used in the study is exclusive and devices are simple and easy to operate. The result is precise and easy to do qualitative analysis of SGR particles, which provides a reliable method to control the quality of SGR particles..The second part Methodological Study on the Content Determination of SGR ParticlesObjective: To control the quality of SGR particles, apply HPLC to determine the contents of ferulic acid(active ingredients of Angelica and Chuanxiong), root of herbaceous peony and Astragalus to determine the safety and effectiveness of SGR particles.Methods:1 Establishment of content determination2 Determine the conditions of using spectrum, adopt appropriate spectrum columns to determine ratio of component, velocity of flow and column temperature3 Methodological studies, determine the content ratio of different herbal medicines.Result:1 Content determination of ferulic acid(active ingredient of Angelica and Chuanxiong). First, in order to determine the content of ferulic acid in Angelica, Column C18 with octadecylsilane bonded silica as fillers,phosphoric acid solution(17:83)with-0.085% acetonitrile as mobile phase are selected. It is found that wave length is 316 nm,column temperature is30℃. UV detector, contrastive spectrum in negative control show the same retention time on spectrum peak. As found in relevant literature, Chuanxiong has a large amount of ferulic acid. The study observes Angelica and Chuanxiong at the same time and detect contrastive ferulic acid solution at the wavelength of 220-400 nm. It is found ferulic acid is absorbed the most amount at the wavelength of 312 nm and 362 nm. The study is not affected by other ingredients in the sample solution with phosphoric acid solution(18:82)with-0.085% acetonitrile as mobile phase, detective wavelength at 316 nm and column temperature at 30℃.Resolution of the main component peak in ferulic acid and its neighboring peak meet the corresponding requirement with good peak shape and retention time. After tested many times, the contents are; there must be at least 0.3mg of ferulic acid extracted from Angelica and Chuanxiong every 1g of SGR particles.2 In order to determine the content of paeoniflorin in root of herbaceous peony, column C18 with octadecylsilane bonded silica as fillers, phosphoric acid solution(14:86)with-0.085% acetonitrile as mobile phase are selected.The wavelength is 230 nm and column temperature is 30℃. UV detector is also used. Mobile phase was changed as phosphoric acid solution(18:82)with-0.1% acetonitrile, but the result was still not satisfactory. Triethylamine was added into 0.1% phosphoric acid solution with a PH value of 5.0.Peak shape of spectrum and retention time was comparatively good. The resolution of peak of main components in paeoniflorin and its neighboring peak meet the requirement. After tested many times, the contents are; there must be at least1.25 mg of paeoniflorin(C23H28O11) every 1g of SGR particles.In order to determine the content of astragaloside in astragalus, column C18 with octadecylsilane bonded silica as fillers, the ratio of acetonitrile to water( 35:65) as mobile phase are selected.The velocity of flow is1.0m L/min and column temperature is 30℃. The injection volume: contrastive control is 10μL and sample 20μL. The velocity of air is 2.5L/min and the temperature of drift tube is 100.0℃. Evaporative light scattering detector is used. The ratio of acetonitrile to water was at first 30:70,32:68.it is found that peaks appear at about 30 and 25 minutes in contrastive control. Acromion appeared in the sample at the same period. It is doubted whether acetonitrile and water have been separated so mobile phase was changed to 35:65. Under this condition, acetonitrile and water have been separated but have not achieved the ideal level so mobile phase was changed into 38:62.Acetonitrile and water have been separated under this condition with optimal result. After about 12 minutes, a peak value appeared with good shape. After tested many times, the velocity of air, the temperature of drift tube was set at2.5L/min and 103.0℃.The change of velocity and temperature affect the peak shape in the spectrum and the accuracy of the research result.After repeated tests, mobile phase was determined: the ratio of acetonitrile and water(35:65),the velocity of flow 1.0m L/min,the temperature of column 30℃. The injection volume 20μL. The velocity of air is 2.5L/min and the temperature of drift tube is 100.0℃. the peak shape of spectrum and the retention time are comparatively acceptable. The resolution of the peak of the main component of astragaloside and its neighboring peak meet the requirement. After tested many times, its content is at least 0.15 mg of astragaloside(C14H68O14) every 1g of SGR particles.Conclusion: To determine the content ferulic acid in(angelica,Chuanxiong), root of herbaceous peony and astragalus, HPLC is adopted. The method is effective, highly sensitive, reliable, precise and stable. It can be used to determine the contents in SGR particles as quality control standards. |
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