RESUMO
Objective To establish a quality control method for detecting impurities in chloral hydrate raw materials, improve the quality standards and control limits of raw materials. Methods The determination methods of chloroform and halogenated carboxylic acid in chloral hydrate were established to monitor the change of impurities in chloral hydrate through stability. Results The research and establishment of chloroform and halogenated carboxylic acid methods met the requirements of relevant regulations for analytical methodology verification, which could accurately detect four impurities in raw materials and preparations by one method. Conclusion The study provides technical support for the improvement and optimization of the quality standards of chloral hydrate and preparations. It is very necessary to implement the impurity monitoring in preparation research and production process by the chloral hydrate impurity detection and the stability comparison of this product at high temperature and light, which could largely promote the safety of medication.
RESUMO
Objective In order to solve the obvious adverse reactions of ribavirin, to develop ribavirin liposome inhalation powder and to evaluate its quality characteristics. Methods The ribavirin liposomes were prepared by the thin film dispersion method, and then lyophilized to prepare ribavirin liposome powder. The appearance, fluidity, bulk density, encapsulation efficiency, particle size of the complex solution, PDI, potential and hydrophilicity were examined. Results Ribavirin liposome powder has good morphology, particle size, potential, fluidity and hydrophilicity, which can meet the basic requirements of powder medicine for drug administration. Conclusion The technique of preparing ribavirin liposome powder aerosol preparation by this method is feasible, and it provides the basic technology for future in vivo and in vitro studies.
RESUMO
Objective To establish a method for the determination of residual solvents in tulobuterol by GC and optimize the purified process of crude tulobuterol product by this method. Methods The analysis was performed on Agilent DB-624 capillary column (30 m×0.32 mm,1.8 μm).The carrier gas was nitrogen at 1 mL·min-1.The injector temperature was 250 ℃.Detector was FID with hydrogen at 45 mL·min-1and air at 450 mL·min-1.The detector temperature was 250 ℃.The column temperature program was used.And the flow ratio was 10:1.Dimethyl sulfoxide (DMSO) was used as solvent of reference and test solution. Results Ethanol,tert-butylamine,dichloromethane,tert-butyl-methyl ether,n-hexane and 1,4-dioxane were completely separated.The calibration curve of each solvent showed good linear correlation. The RSD of precision was less than 5.0% and the average recovery ranged from 97.0% to 104.0% (RSD<5%).By optimizing the purification process of toloterol,the residue of organic solvent in the preparation of tolobuterol was in accordance with the Chinese Pharmacopoeia ( 2015) limit. Conclusion Validated by methodology,this simple,rapid and precise method can be used for the test of residual solvents in tulobuterol.
RESUMO
OBJECTIVE:To prepare borneol-modified colchicine ethosome,and to evaluate its in vitro transdermal permeation. METHODS:Borneol-modified colchicine ethosome was prepared with ultrasonic injection-probe ultrasonic method,and its ethosome was characterized. The content and moditication rate of borneol in borneol-modified colchicine ethosome was determined by GC;content and encapsulation rate of colchicine was determined by HPLC.Accumulative permeability and permeation rate were investigated for colchicine ethanol solution,colchicine-borneol-ethanol solution,colchicine ethosome without borneol-modification, borneol- modified colchicine ethosome after diffused for 1,3,6,8,12,16,24,48 h. RESULTS:The average particle size of borneol- medified colchicine ethosome was about(110.4 ± 5.1)nm,polydispersity index was 0.110 ± 0.030,Zeta potential was (2.33±0.20)mV,prepared ethosome is approximately spherical in shape and multilaminar vesicles in structure. Encapsulation rate of colchicine was 56.12%,and modification rate was 9.85%. The in vitro diffusion tests showed that after diffused for 48 h, accumulative permeability per unit area of borneol-modified colchicine ethosome was 103.52 μ g/cm2;permeation rate was 1.26 times as colchicine ethosome without borneol-modification,1.77 times as colchicine-borneol-ethanol solution and 5.14 times as colchicine ethanol solution. CONCLUSIONS:Prepared borneol-modified colchicine ethosome has small particle size,narrow particle size distribution,high modification rate and good transdermal permeation.
RESUMO
Objective To establish a mini-column centrifugation-HPLC method to determine the entrapment efficiency of levodopa-loaded PEGylated-solid lipid nanoparticles.Methods A dextran gel(Sephadex G-50) mini-column centrifugation was employed to separate the free drug from solid lipid nanoparticles.The content of levodopa was qualified by HPLC.Results Under the applied chromatographic condition,the excipients had no influence on the determination of levodopa.A calibrated linear of levodopa concentration was within 10.54-527.00 μg·mL-1.The recoveries of high,medium and low concentrations of levodopa were 99.13%,99.51% and 99.04%(RSD were 1.25%,1.91% and 1.71%), respectively.The free levodopa was well separated from solid lipid nanoparticles by using mini-column centrifugation.The addition of blank solid lipid nanoparticles recovery was 98.84% with RSD of 0.80%(n=3).The average adsorption rates of the three concentrations of free levodopa were 100.00%,98.75% and 98.56%(RSD were 0.00%,0.19% and 0.18%,n=3),respectively.The adsorption rate of the physical mixtures of three different concentrations of drugs and empty PEGylated solid lipid nanoparticles were 99.68%,98.46% and 99.21%(RSD were 1.52%,0.23% and 0.21%),respectively.Conclusion The method was simple,accurate and reproducible,which can be used for determination of the entrapment efficiency of levodopa-loaded PEGylated-solid lipid nanoparticles.
RESUMO
Objective: To develop 5-FU multiple emulsion entrapped into thermo-sensitive gel (5-FU-DEG) and detect the ab-sorption and transportation in Caco-2 cell monolayer model. Methods:The 5-FU multiple emulsion was prepared by a two-step emulsif-ying method. Poloxamer 407 (P407) was used as the thermo-sensitive material and sodium alginate (SA) was used as the bioadhesive material for the preparation of 5-FU-DEG. Caco-2 cell monolayer model was used to investigate the transportation and absorption of 5-FU. Results:5-FU-DEG gelled at the ambient temperature and turned into liquid below 10℃ The apparent permeability coefficient (Papp) of 5-FU-DEG was 1.47 ±0.11 ×10 -5(cm·s-1), which was about 6 times higher than that of 5-FU water solution(2.39 ± 0.21 ×10 -6 cm·s-1)(P<0.01). The cellular uptake rate of 5-FU-DEG was (17.1 ±0.24) %, which was 3.9 times greater than that of 5-FU water solution (4. 41 ± 0. 23%)(P<0. 01). Conclusion:5-FU-DEG can efficiently enhance the transportation and ab-sorption of drug in rectal site by using micro-emulsion technology combined with thermo-sensitive technology, which can be an effective rectal delivery system for 5-FU to treat rectal cancer.
RESUMO
Objective To establish a HPLC method for determination of related substances of risedronate sodium tab‐lets .Methods The C18 column ,5 μm ,150 mm × 4 .6 mm ,the buffer solution (3 .22 g tetrabutyl ammonium bromide was added to a buffer solution of 1 000 ml 0 .05 mol/L ammonium chloride ,then adjusted pH to 7 .8 ± 0 .05 by ammonia)‐methanol‐aceto‐nitrile =250:50:25 as mobile phase ,column temperature:room temperature ,flow rate:1 .0 ml/min ,detection length:254 nm . Results Determined by HPLC at high temperature ,acid ,alkali degradation ,the main peak and the impurity peaks were separa‐ted well ,and the peaks had a linear relationship ,Y=1 .28 × 107 X-1 .62 × 105 (r=0 .999 9) .Conclusion The method was rap‐id ,simple ,accurate and sensitive ,and suitable for determination of risedronate sodium tablets related substances .
RESUMO
Objective:To establish a method for determining three residual organic solvents in nimodipine liposomes. Methods:The samples were injected into a DB-624 capillary column (30 m × 0. 32 nm,1. 8 μm) by a headspace sampler and analyzed with an FID detector, the carrier gas was nitrogen, the injector temperature was 250℃, and the detector temperature was 250℃. The column temperature was programmed raised. Results:Three residual solvents, namely ethanol, acetone and acetic ether were completely sepa-rated. There was a good linearity within the experimental concentration range. The average recovery was 98. 9%,98. 5% and 99. 4%(RSD=0. 32%,1. 12%,0. 76%,n=9), respectively. The detection limits was 0. 20, 0. 18 and 0. 22μg·ml-1, respectively . Con-clusion:The method is rapid, sensitive and accurate. It can be used in the determination of residual organic solvents in nimodipine li-posomes.
RESUMO
Objective:To establish an HPLC method for determining the contents of related substances in vinpocetine injections. Methods:The chromatographic separation was performed on a Kromasil C18 column (150 mm × 4. 6 mm,5 μm). The mobile phase consisted of 0. 2 mol·L-1 ammonium acetate -acetonitrile (40∶60), the flow rate was 1. 0 ml·min-1, the detection wavelength was 280 nm,and the injection volume was 20μl. Results:Vinpocetine and the related substances such as ethyl vincaminate, apovincamine, methoxyvinpocetine and dihydrovinpocetine were separated completely. The calibration curves of related substances showed good linear-ity. The average recoveries of related substances were all above 99. 8%. Conclusion:The method is accurate, sensitive and specific, and can be applied in determining the related substances in vinpocetine injections.
RESUMO
Objective:To investigate the effects of various bio-adhesive polymers on bio-adhesive characteristics and release rate of 5-fluorouracil HP-β-CD inclusion complex thermo-sensitive gels. Methods: Bio-adhesive polymer, such as hydroxypropylmethylcellu-lose ( HPMC) , sodium alginate ( SA) , sodium hyaluronat ( HA) ,carbopol and polycarbophil was respectively used to prepare the ther-mo-sensitive gels, and the bio-adhesive force was studied. The phosphate buffer (pH 7. 2) was used and the drug release characteris-tics were studied using dialysis technique. Results: The bio-adhesive force of the gels with 0. 2% polycarbophil was 32. 3 g·ml-1 , and the drug release time was prolonged to 8 h. There was no obvious difference in the dissolution among the gels with the various bio-adhesive polymers. Conclusion:Using 0. 2% polycarbophil as the bio-adhesive polymer, 5-fluorouracil HP-β-CD inclusion complex thermo-sensitive gels show good bio-adhesive force and prolonged drug release characteristics.
RESUMO
Objective To establish a method for determination of imatinib mesylate liposome and related substances. Methods The liquid chromatography was carried out on a Kromasil C18 column. The mobile phase A consisted of methanol-octane sulfonate solution(42:58). The mobile phase B consisted of methanol-octane sulfonate solution(4:96). The flow rate of gradient elution was 1. 2 mL·min-1 . The detection wavelength was 268 nm. The column temperature was room temperature. Results The intermediates and degraded substances could be seperated under the selected chromatographic conditions. Imatinib mesylate showed a good linear relationship within 1-100μg·mL-1,r=0. 999 1(n=5). Conclusion The method is specific, accurate,sensitive,and simple,and can be used for quality control of imatinib mesylate liposome.