| ObjectivesJinggu tablet derived from the classical prescription "Jinggu pill", which was recorded in Ru Men Shi Qin. Sophora japonica and Fructus aurantll are its main prescription. As classic couplet medicines, they have been the core of anti-hemorrhoid medicines, such as fructus sophorae pill. Besides, rutin and naringin, the main components of Jinggu tablet, have significant anti-inflammatory and anti-microcirculation function. This thesis focuses on the study of the preparation technology and quality standard of Jinggu tablet.MethodsStudy on preparation process of Jinggu tablet: This thesis researched the extract of Jinggu prescription as well as excipients and coating in the tablet process of Jinggu tablet, then studied pilotscale experiment respectively. 1. Extract was obtained by water extraction, ethanol precipitation and drying of crude drugs in Jinggu prescription. Taking the total flavonoid content as an indicator, with orthogonal experimental design, the author optimized the additive water added, extraction time, times of extraction and grinding degree in water-extracting technology and optimized the concentrate rate, the concentration of the ethanol and static time in ethanol precipitation technology after the extraction. After that, the author, taking sample’s water content and flavonoid content as an indicator, studied the temperature and time of drying in drying technology. 2. The direct powder compression method was adopted to respectively filtrate the types and dosage of excipients, excipients proportioning, the types and dosage of disintegration mainly according to liquidity and compressibility, tablet disintegration time limit, hardness and brittle broken degrees.Also thin film coating of tablet coating fluid formula, coating and coating weight were investigated and researched.Studied on quality standard of Jinggu tablet: Qualitative and quantitative analysis of Jinggu tablet’s quality were carried out by thin layer chromatography(TLC), UV spectrophotometry and HPLC method respectively. 1. TLC method was adopted for qualitative identification of Jinggu tablet, with silica gel G plates thin layer plate, ethyl acetate:formic acid:water(8:1:1) as developing system, and aluminium chloride solution as chromogenic reagent, examining under 365 nm. 2. Using UV spectrophotometry, with rutin as reference substance, determined flavonoids in the samples were determined at the wavelength of 257 nm. 3. HPLC method was established for simultaneously determination rutin, naringin, hesperidin, neohesperidin and quercetin in Jinggu tablet. The analyte was performed on Elite Kromasil-C18 column(4.6 mm×250 mm, 5 mm), and the mobile phase consisted of acetonitrile-0.2% acetic acid. The flow rate was 1.0 m L/min and detection wavelengths were set at 254 nm for rutin and quercetin, 283 nm for naringin, hesperidin and neohesperidin.ResultsPreparation process of Jinggu tablet showed: 1. preparation technology of the extract of Jinggu prescription was: hovenia dulcis(coarse particle) and sophora japonica(Fried) were refluxed 12 times the amount of water for 3 times, 2 hours each time. Then mixed up the whole extract of the 3 times and concentrated to the volume twice the size of the original crude drugs(volume and weight ratio: m L/g). The condensed extract was then added appropriated amount of ethanol to make the ethanol concentration of the solutionto is 70% and leave to stand for a night. Then supernatant were collectd, decompressed(55 ~ 60 °C, 0.09 ~ 0.10 MPa) and concentrated it(the proportion is about 1.25 g/cm3) and dried in vacuum for 12 h(0.09~0.10 MPa vacuum degree) at 60 °C. The data of pilotscale experiment agreed with laboratory experiment, and the repeatability was good. 2. Pharmaceutical process:Raw excipients respectively through 80 mesh sieve, lactose: microcrystalline cellulose: crosslinking povidone mix: magnesium stearate: powder silica gel(50.0: 16.6: 30.0: 2.0: 0.7: 0.7) were mixed up and compressed to tablet directly; Then make 16% of the coating solution, Following which, preheat tablet in the oven to 40~50 °C, make the temperature of tablet bed in coating pot rise to about 70 °C, open spray gun. In the process of making initial coating, the rotating speed of coating pot is 0.8~4 r/min, and the flowing speed of spray gun should be controlled in 2~6 m L/min. When the core of tablet is covered a thin layer of membrane, gradually speed up the coating pot and the spray gun: coating pot’s speed should be 5~13 r/min and spray gun’s 7~15 m L/min; The coating process won’t be stopped until the core of tablet gain the weight of 2.86%; Put the coated tablet in 50 °C oven and solidify for 1 hour; Qualified tablet with a thin coating comes. The pilotscale experiment was smoothly, good reproducibility, and The quality indexes inspection were qualified.The results of the study on Jinggu tablet quality standard shows: 1. The Jinggu tablet of TLC identification results showed that in the chromatogram of the test, the control medicinal materials or reference substance chromatography corresponding position, rutin and naringin spots were clear, and the negative control without interference in their place. 2. UV determination results showed that flavonoids content of Jinggu tablet in 4.89 mg/m L~24.44 mg/m L has a good linear relationship(r = 0.9999), the method of average sample recovery rate was 97.37%, RSD was 0.22%.And the flavonoids of Jinggu tablet was 39.00mg/tablet; 3. HPLC determination results showed a good relationship in the ranges of 0.0125-0.5004 g/L for rutin, 0.0100-0.4008 g/L for naringin, 0.0033-0.0327 g/L for hesperidin, 0.0113-0.2256 g/L for neohesperidin and 0.0041-0.0813 g/L for quercetin. All of the average recoveries were between 98% and 102%. And the content of rutin, naringin, hesperidin, neohesperidin, quercetin in Jinggu tablet were 9.40 mg/tablet and 4.67 mg/tablet and 0.41 mg/tablet and 3.81 mg/tablet, 0.92 mg/tablet.Conclusions1. The preparation technology of the extract of Jinggu prescription is easy, stable and reliable; 2. Tablet friability and hardness of finished tablet which is made by optimized pharmaceutical technology is desirable, which shows that the technology is steady and its formula design is reasonable; 3. TLC method demstrates that rutin and naringin in Jinggu tablet have a good reproducibility and their specificity is strong. Thus, this method can be used as an identification method for Jinggu tablet; 4. Regard to determination of UV and HPLC, the operation is simple, the result is accurate and reliable, and the feasibility and repeatability is good. Therefore, they can be employed as the quality control method of Jinggu tablet.This paper mainly about Jinggu tablet of preparation technology and quality standard, provide some basic data for the research and development of Jinggu tablet. |
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