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12The proportions of elderberry prescription glycosides with lactose, MCC, PVPP mixing, granulating 70% ethanol, dried, whole, plus magnesium stearate, mixing, tabletting. Examine tablet weight variation, disintegration time, friability, hardness. Experiment 3 batchesD Table 6 The verification results of preparation process
Experime nt No. Weight difference Disintegratio n time Friability (%) Hardness (kg.cm-1)
1 0.3615±0.05 17 0.6 3.6±0.2
2 0.3594±0.08 19 0.6 3.5±0.2
3 0.3611±0.04 16 0.5 3.8±0.1
The results showed that the average tablet weight of the preparation, disintegration time, friability, hardness are in line with the requirements under pharmacopoeia tablets, process stability, can be used as total jiegumu glycosides tablet formulation process.
Conclusions
Determine the preparation process:total jiegumu glycosides 32g,lactose 288g,MCC 32g, PVPP 7g full mixing, over 80 mesh sieve, soft material made of 70% ethanol, 20 mesh sieve granulation, drying, whole, plus stearin magnesium 3.5g,mix make total jiegumu glycosides tablet.The research of total jiegumu glycosides tablet that is the preparation technology scientific and stable .The chip can develop total jiegumu glycosides tablet and provide the basis for new drugs.
References
1.Jiangsu New Medical Editor. Chinese Dictionary (two volumes) [M]. Shanghai Science and Technology Press, 1985:2093.
2. Zhao Xiaohong, Chen Di hua, SI Jian-yong, etc. Traditional Chinese Drug Research tablet formability ideas and methods [J] Chinese Journal of Clinical Pharmacology, 2002,13 (5) :327-329.
3. Armando Caceres, Brenda R. Lopez, Melba A. Giron and Heidi Logemann. Plants used in guatemal for the treatment of dermiatophytic infection. 1.screening for antimycotic activity of 44 plant extracts. Journal of Ethnopharmacology, 1991, 31(3): 263-276.
4. Liu Zheng, Wu Jingsheng, Wang Minwei. Elderberry oil lipid-lowering and anti-aging effect of [J]., Shenyang Pharmaceutical University, 1995, 12: 127-129.
5. Mlinaric A, Kreft S, Umek A, Strukelj B. Screening of selected plant extracts for in vitro inhibitory activity on HIV-1 reverse transcriptase(HIV-1 RT). Pharmazie,
Study onQuality Standard of Total Jiegumuglycosides tablet
LU Qing-xiu,Yang Liu, Jiang Hai,Wang Qiu-hong, Yang Bing-you, Kuang Hai-xue*
Key Laboratory of Chinese Materia Medica,Heilongjiang University of Chinese Medicine,Ministry of Education,Key Laboratory of Traditional Chinese Medicine and Natural Medicine Pharmacodynamic Material Base,Harbin 150040, China
Abstract:Objective: To study the quality standard of total jiegumu glycosides tablet.Method: Ast ragalus morroniside were identified by TLC method;The content of total jiegumu glycosides tablet was determined by HPLC and determine the dissolution of morroniside in total jiegumu glycosides tablet by slurry. According to the 2010 edition of "Chinese Pharmacopoeia"provisions of the relevant tablets, firstly, we established inspection methods of
weight difference, disintegration, heavy metal, arsenic salt and microbial limit oftotal jiegumu glycosides tablet. Result: TLC method can well identify morroniside, liquid negative control without interference; Determine the detection limits of morroniside is no less than 4.0% in HPLC;precision was 3.206%, stability was 2.776%, and repeatability of 1.427%, the average recovery was 99.63%. Establish methods are accord with pharmacopoeia. Conclusion: The analysis method was accurate, reliable, well meet the requirement of analysis methods of the analysis.
Key words:total jiegumu glycosides tablet; morroniside; TLC
Sambucus williamsii Hance(jiegumu) derived from Sambucus species of Caprifoliaceae [1].The main efficacies of jiugumu include fractures, bruises, swelling and bleeding trauma [2] Accoarding to the preliminary studies of task Force [3,4],The root of jiegumu have significantly promote fracture healing, and to clarify the material basis for total jiegumu glycosides. Task Force will total jiegumu glycosides prepared into tablets for clinical patients taking. In order to control the quality of total jiegumu glycosides tablets to ensure safe and effective of clinical use drugs,the paper established the quality standards of total jiegumu glycosides tablets.
Materials
Waters-2695 HPLC;SB-5200D ultrasonic cleaner (Experimental Instrument Factory Co., Ltd. Ningbo); electronic analytical balance (Switzerland METTLER TOLEDO company). Morroniside reference substance, (the purity of morroniside was determined to be more than 98%); total jiegumu glycosides tablets, Heilongjiang University of Chinese Medicine Department of Chemistry homemade (batch number: 20100001,20100002,20100003,0.36g/piece);methanol was of analytical grade (U.S. DIKMA company); other solvents were of analytical grade.
Methods and Results
1.The TLC of Morroniside
1.1The preparation of reference substanceN the test and negative control solution.reference substance:Accurately weighed morroniside reference substance 25mg, add methanol made 5mg/ml solution. The test solution : Weigh total jiegumu glycosides tablet 0.1g, add methanol 10ml, ultrasonic treatment 30min, filtration, as the test solution. Preparation of the negative control solution : Accoarding to the prescription weigh other excipients into tablets except total jiegumu glycosides (total jiegumu glycosides 32gN lactose 288gN MCC 32gN PVPP 7gN magnesium stearate 3.5g, In accordance with the test operation is made under the negative control solution
1.2TLCIn accordance with the 2010 edition of "Chinese Pharmacopoeia" thin-layer chromatography test, draw the three solutions 5^1, Point in the same silica gel GF254 TLC plate, With chloroform - methanol (3:1) as developing solvent, Under the UV lamp view (254nm) .Test products for chromatography, chromatography with reference substance corresponding position was the same purple spots. While the negative is no reference standard chromatographic blank spots.
1.3 The content determination of morroniside.Selecting morroniside as the index components of total jiegumu glycosides tablet was measured by HPLC,and make the appropriate methodological study.Chromatographic conditions:Co1umn:Diamonsi1 C18 co1umn(250mm*4.6mm ID,5^,,Dima company),mobile phase:methanol-water(30:70v/v) detection wavelength:240nm,flow rate:1.0m1/min,co1umn emperature:room temperature,injection vo1ume:10piDetermination:the reference solution, the test solution and the negative control solution was prepared with1.1. The precise amount of the above-mentioned three kinds of solution into the liquid chromatograph, record the chromatogram peak area of morroniside.
2 The study of methodology
2.1The interference investigation of negative sample The reference solution and the negative contro1 so1ution 10pl,into the 1iquid chromatograph, the resu1ts show that negative contro1 so1ution without interference.
2.2 Linear Relation
Taking the above 0.1,0.3,0.5,0.7,0.9,1.2mg/ml concentration of six standard solutions, respective1y, samp1e 10p1 Measured peak area to reference content X is the abscissa and peak area Y is the vertical axis, the standard curve. The regression equation: Y = 2.012x106X+600633(R2=0.999),indicate the reference range at 1^g~12^g was good 1inear relationship.
2.3 For precision, stability, reproducibility, recovery test results show that precision was 3.206%, stability was 2.776%, and repeatability of 1.427%, the average recovery was 99.63%,RSD was 1.43%.
2.4Determination of sample formulation with content limits Taken 10 batches of total jiegumu glycosides tablet,according to the method of 2.2,prepared for the test solution,measured the content of morroniside.The results showed that the content of morroniside in tablets was stable basically,the average content of morroniside is 4.595%, therefore limited morroniside content was no less than 4%.
3 Determination of Dissolution
3.1 Determination of the dissolution curve
Lot number t (min)
15 20 30 45 60 75
20100001 41.5 81.6 92.4 101.6 102.4 102.3
20100002 39.7 79.8 93.1 100.8 102.1 102.8
20100003 42.3 80.4 90.5 99.7 101.3 101.9
Table1 The measurement results of morroniside dissolution profile in3 batches total jiegumu glycosides tablet
Determined dissolution of total jiegumu glycosides tablet with the slurry and distilled water after degassing as the dissolution medium,the volume selection 900mL, speed is 100r/min, temperature of 37 °C, according to the operation. Taking 5ml samples respectively in15,20,30,45,60,75min,0.45^m microporous membrane filtration, adding the same volume of dissolution medium at the same temperature. Determination the absorption of morroniside at 240nm by HPLC,calculated cumulative dissolution rate.The dissolution of total jiegumu glycosides tablet can reach 90% in 30min.
4 Detection
4.1 Weight difference
Sample batches Standards Differences range Conclusion
20100001 <±5.0% -3.69%—3.57% Compliance
20100002 -3.46%—3.73% Compliance
20100003 -3.55%—3.81% Compliance
Table3 The measurement results of weight variation in three batches of total jiegumu glycosides tablet
Accordance with the "Chinese Pharmacopoeia" 2010 edition an appendix I General tablet formulations under inspection methods and standards.The average piece of three batches samples, was 0.36g so, the difference does not exceed 5.0%.Meet the pharmacopoeia requirements.
4.2 Disintegration
Accordance with the "Chinese Pharmacopoeia" 2010 edition an appendix M A disintegration test method checks.Conducted 3 batches of tests, the results in Table 4
Sample batches Disintegration time (min)
20100001 13 14 15 12 11 14
20100002 16 15 14 18 11 14
20100003 16 14 15 15 14 12
Table 4 3 The measurement results resultsbatches of disintegration in three total jiegumu glycosides tablet
Table 4 shows,all three batches of samples for the test were disintegration time of 20 minutes or less.Meet the Pharmacopoeia requirements.
4.3 Heavy metals Take this product 2g, a small fire burning charcoal,burning ashed at 550°C.The precise amount of lead solution 2ml,in accordance with the "Chinese Pharmacopoeia" 2010 edition an appendix K E (second method) inspection method for detecting heavy metals, experimental three batches of samples containing heavy metals did not exceed ten millionths.
4.4 Arsenic Take this product 1g, 2g arsenic plus calcium hydroxide,a small fire burning charcoal,burning ashed at 550 ° ,with hydrochloric acid were neutral as the test solution.The precise amount of arsenic solution 2ml, the same treatment as a control solution. Accordance with the "Chinese Pharmacopoeia" 2010 edition an appendix K F (first method) Arsenic inspection method for detecting the experimental three batches of samples, were not more than two millionths of arsenic.
4.5Microbial Limit
Sample batches Total number of bacteria (Cell s/g) Fungal / yeast count (Cells/g) E. coli Live mites
20100001 460 0 Undetected Undetected
20100002 370 0 Undetected Undetected
20100003 450 0 Undetected Undetected
Table5 The test result of microbial limit in 3 batches total jiegumu glycosides tablet
Accordance with the "Chinese Pharmacopoeia" 2010 edition an appendix MI C microbial limit test method for detecting, from Table 5, three batches of samples are in compliance with Pharmacopoeia requirements.
Discussion
There are two methods dissolution, respectively, and the rotating basket method slurry method [5], the measurement morroniside dissolution curve, the slurry method is better than the rotating basket dissolution method, Slurry method was chosen determination dissolution.
References
1. Jiangsu New Medical Editor. Chinese Dictionary (two volumes) [M]. Shanghai Science and Technology Press, 1985:2093.
2. Han Hua, Yan Xueying, Marina Hai, etc. elderberry Research Progress [J] Medicine Information, 2008,25 (6) :14-16.
3. Lu Fang. Thesis "elderberry chemical constituents of the root bark" Heilongjiang University of Chinese Medicine, 2002.
4. Han Meihua. Thesis "elderberry root bark chemical composition and its compound preparation molding process of" Heilongjiang University of Chinese Medicine, 2003.
5. Chinese Pharmacopoeia. A [S] .2010.
Research the effect of Sambucus glycosides tablet on bone fracture healing
Ya-wen HE, Liu YANG, Hai JIANG, Qiu-hong WANG, Bing-you YANG, Hai-xue KUANG* Heilongjiang University of Chinese Medicine, Harbin, China
Abstract: Objective To reach the effect of Sambucus glycosides tablet on bone fracture healing following bone injury and its mechanism. Methods Fractures were made in the left tibiae of male New Zealand White rabbits. The fractures were made using the technique of incomplete fracture. Sambucus glycosides tablet were administered (each group at 220, 110 and 60 mg/kg doses) orally to adult Rabbits. After 12, 24, 36 days of treatment, animals were administration of marginal ear vein blood. Determination of the serum BGP, ALP, Ca2+ and P changes with determination kit. By X-ray extent of fracture healing observed in each group. After the last dose, euthanized and femur bones collected, With DEXA bone mineral density tests were performed in order to determine bone mineral density (BMD), bone mineral content (BMC) and callus area. Detect TGF-pi, BMP-2, Col- I a1 and Col-Ha1 mRNA expression in fracture healing each period using reverse transcription - polymerase chain reaction and real-time fluorescence quantitative method. Results Sambucus glycosides tablet on fracture rabbit serum ALP, serum BGP, serum P levels were significantly increased, serum Ca2+ concentration decreased; fracture zone of rabbit bone density, bone mineral content, bone callus area has significantly increased role. X-rays showed elderberry total glycosides tablet may promote healing of the fracture zone. Elderberry total glycosides tablet in fracture healing process of the BMP-2, TGF-P1 had no significant effect, can promote the expression of Col- I a1, inhibit the expression of Col-Ha1. ConclusionSambucus glycosides tablet can promote rabbit fracture late maturation and calcification of bone matrix; promote collagen synthesis and deposition of calcium salts; improve quality of callus; accelerate fracture healing.
Keywords: Sambucus glycosides tablet; fracture healing; mechanism
With bone fracture emerged as one of the most important health issues, more and more investigations are focusing on bone fracture healing. Fracture healing is a complex cascade of cellular events and the regulation of its healing remains poorly understood. Large number of clinical observations suggest that Sambucus treatment of fractures has a characteristics of short duration, rapid recovery and high efficacy.However, there are few studies on the mechanism of fracture healing.
Materials and methods
Fractures were made in the left tibiae of male New Zealand White rabbits weighing approximately 2.5 kg.The operations were performed under sterile conditions. The rabbits were anesthetized with Sodium pentobarbital. The fractures were made using the technique of Incomplete fracture.Sambucus glycosides tablet were administered (each group at 220, 110 and 60 mg/kg
