ABSTRACT
Objective: To prepare the new diclofenac potassium cataplasms, establish a quality research method and evaluate the preparation quality by the established method. Methods: A high performance liquid chromatography(HPLC)was performed on an ODS column(the column temperature 35℃)using the methanol-4% glacial acetic acid solution(80: 20, V/V)as mobile phase, and the detection wavelength was set at 276 nm. Diclofenac potassium was extracted with methanol, and the adhesion, content and uniformity of potassium diclofenac were measured. The release of diclofenac potassium from the cataplasms was determined in accordance with the fourth method of the XD release methods in the Appendix of the Chinese Pharmacopoeia. Results: The average maximum number of steel ball stuck in the cataplasms in the initial adhesion test was No. 6. Under the HPLC conditions, potassium diclofenac showed good linearity within the concentration range of 400-800 μg/ml, with the average sample recovery rate 1.33 % and RSD< 1.93%(n=6). The methodological studies for the drug release test for the diclofenac potassium cataplasms showed that the diclofenac potassium showed a good linearity within the range of 1-50 μg/ml in the drug release test, and the precision and recovery well satisfied the requirements of Pharmacopoeia. The content uniformity of the cataplasms was in accordance with the Pharmacopoeia. The release amounts of the cataplasms in 2, 5 and 8 hours were 20%-45%, 40%-80% and more than 70% of the labeled amount, respectively, and the release curve followed the first-order release equation. Conclusion: The established HPLC method is sensitive, accurate, easily operable and reproducible, which could be used for the quality control of diclofenac potassium cataplasms. The prepared diclofenac potassium cataplasms were of uniform content and showed characteristics of the sustained release, which is expected to be developed to a new preparation of diclofenac potassium.
ABSTRACT
Objective: To establish a GC method for the determination of content and content uniformity of memantine hydrochloride dispersible tablets.Methods: The sample was dissolved in water, alkalified by sodium hydroxide solution and extracted by methylene chloride.An HP-5 gas chromatography column (50 m×0.32 mm, 1.05 μm) was used.The column temperature was programming increased, and the initial temperature maintained at 120 ℃ for 3 min, and then raised to 220 ℃ at a rate of 10℃·min-1 and maintained for 7 min.A hydrogen flame ionization detector (FID) was used and the split ratio was 1∶1.The inlet temperature was 230 ℃ and the detector temperature was 260 ℃.The injection volume was 1 μl and the carrier gas was nitrogen with high purity at a flow rate of 3.0 ml·min-1.Adamantane was used as the internal standard, and the internal standard method was used for the calculation.Results: The calibration curve was linear over the range of 0.05-1.0 mg·ml -1 (r=0.999 7).The detection limit and the limit of quantification was 1.1 ng and 3.3 ng, respectively.The average recovery was 100.2% (RSD =0.73%, n=9).Conclusion: The method has the advantages of simple operation, small extraction process toxicity, little environmental pollution, high accuracy and high specificity, and can be used for the determination of content and content uniformity of memantine hydrochloride dispersible tablets.
ABSTRACT
Objective To prepare nasal triptolide nano liposome thermosensitive gel (TP-NLS-TG) and investigate the in vitro penetrability through nasal mucosa. Methods The triptolide nanoliposomes were prepared by high pressure homogenization method, and the ratio of poloxamer 407 (P-407) and poloxamer 188 (P-188) was selected, using the azone dosage and stirring time as investigation factors. Gelation temperature (GT) and homogeneity of TG (RSD) were used as evaluation indexes, and TP-NLS-TG was prepared by optimized prescription. An isolated mucosal permeability model was established by frog abdominal skin to carry out the in vitro permeation test of TP-NLS-TG in nasal mucosa. Results The best prescription was 12% P-407, 10% P-188, and 3% azone, and swelling time was 4 h. The TP-SLN gelation temperature of the gel was 32 ℃, and the RSD was 0.005%. In the first 8 h, the cumulative infiltration volume per unit area was (9.296 3 ± 0.614 7) μg/cm2, and the release curve in line with the Higuchi mathematical model. Conclusion The triptolide nano liposome gel prepared by the optimum technology has an accurate gelling temperature, and uniform content, which has good permeability, can be absorbed through the frog skin.
ABSTRACT
OBJECTIVE:To establish a method for the determination of content and content uniformity in Bisacodyl enter-ic-coated tablet. METHODS:HPLC method was performed on the column of Agilent ZORBAX C18 with mobile phase of acetoni-trile-20 mmol/L ammonium acetate(adjusted pH to 5.0 with acetic acid)(55∶45,V/V),the detection wavelength was 265 nm,col-umn temperature was 30℃,flow rate was 1.0 ml/min,and the volume injection was 20 μl. RESULTS:The linear range of bisaco-dyl was 50-1 000 μg/ml(r=0.999 9);RSDs of precision,stability and reproducibility tests were lower than 1%;recovery was 99.50%-101.17%(RSD=0.5%,n=9). CONCLUSIONS:The method is reproducible with high accuracy,and suitable for the quali-ty control of Bisacodyl enteric-coated tablet.
ABSTRACT
To establish an HPLC method for the determination of content and content uniformity of minoxidil tablets. Methods:An Xbridge C18 column (250 mm ×4.6 mm, 5 μm)was used with methanol-0.03 mol·L-1 KH2PO4 solution -triethyl-amine(60∶40∶0. 1)(adjusting pH to 3. 5 with phosphoric acid ) as the mobile phase. The flow rate was 1. 0 ml·min-1 and the detec-tion wavelength was 287 nm. The column temperature was 30℃ and the injection volume was 10 μl. Results:There was a good linear relationship within the range of 8. 056-32. 224 μg·ml-1(r=0. 999 9). The average recovery was 99. 68%(RSD=0. 36%,n=9). The average content of 3 batches of samples was 100. 2%,100. 5% and 99. 8% and the content uniformity was 5. 5,6. 2 and 4. 9, re-spectively. Conclusion:The method is simple and accurate with good reproducibility, which can be used in the quality control of mi-noxidil tablets.
ABSTRACT
Objective:To establish a method for the content uniformity ( CU) of fennel oil in Weitongning tablets to study the CU of fennel oil in Weitongning tablets. Methods: Methyl salicylate as the internal reference, the content of trans-anethole in fennel oil was determined by GC. The separation was performed on a DB-FFAP capillary column (30 m × 0. 32 mm, 0. 25 μm) at 145℃, the injection part temperature was 180℃ and the FID detector temperature was 230℃, nitrogen with high purity was used as the carrier gas at the flow rate of 0. 8 ml·min-1 . The air flow rate was 400 ml·min-1 and that of hydrogen was 35 ml·min-1 . The methodology validation was carried out, and the samples from different companies with different batches were determined. Results:Significant differ-ence showed in the CU of fennel oil in the samples with different batches from the same manufacturer or from different companies. The trans-anethole showed linear correlation within the range of 2. 189-35. 030 μg · ml-1 ( r =0. 999 9 ) and the average recovery was 100. 06% (RSD=0. 5%, n=9). Conclusion:The method is simple and quick. It is accurate in the CU determination of fennel oil and can be used for the quality control of Weitongning tablets.
ABSTRACT
Objective:To establish an HPLC method for the content determination of gliquidone tablets to improve the specificity of the content determination and the rationality of the preparation of test solution. Methods: A UPLC-MS system was used to analyze the degradation products with positive and negative ion scanning and sub-ion scanning. An ACQUITY UPLC BEH C18 column(2. 1 mm × 50 mm,1. 7 μm) was employed with the mobile phase consisting of water (adjustting pH to 3. 5 with formic acid)-acetonitrile with gradient elution. The HPLC method was performed on an Agilent Zorbax SB-C18 column(150 mm × 4. 6 mm,5 μm). Water (adjusing pH to 3. 5 with formic acid)-acetonitrile(37. 5∶62. 5) was used as the mobile phase. The detection wavelength was set at 230 nm. The column temperature was set at 30℃. The flow rate was 1. 0 ml·min-1 with the injection volume of 20μl. Results:A good linear re-lationship was obtained within the range of 60. 200-140. 400μg·ml-1(r=0. 999 5), and the average recovery was 98. 60% with RSD of 0. 6% (n=9). Conclusion:The method is accurate, reliable, specific and reproducible, which can be used in the determination of content and content uniformity of gliquidone tablets.
ABSTRACT
This study was aimed to introduce the key link in the process of granulating of small-dose methyl can-tharis amine tablets. Combined with practical experiences in daily jobs, related literatures in recent years from the fineness of raw materials, choice of main materials mixing, selection of adhesive, drying methods and grain quality were analyzed. The results showed that in order to ensure the content uniformity of small-dose tablets and conform to requirements of the Chinese Pharmacopoeia, the fineness of raw materials should be appropriate; the main supple-mentary material must be evenly mixed with enough time; the choice of adhesive should be scientific and reasonable;the drying method should be practical; and the grain quality should meet the technological requirements.
ABSTRACT
In this paper, the essentiality of content uniformity of Chinese materia medica (CMM) is taken as a breakthrough point, the determination and assessment methods which may be used for the content uniformity of CMM are summarized, and the measures respected by author of IR fingerprint and machine vision technology are elaborated, in order to enhance the quality of CMM preparations, strengthen the safety and effectiveness of clinical medicine, and promote the establishment of content uniformity evaluation system suitable for CMM preparations.
ABSTRACT
The aim of the present work was to develop simple, shorter and effective HPLC method with UV detection (285nm) and subsequent validation for the content uniformity determination of Rabeprazole Sodium in marketed tablet samples. The method uses isocratic mobile phase of 0.1M sodium phosphate buffer (pH adjusted to 6.5 with sodium hydroxide solution) and acetonitrile 65:35 compositions on reverse phase Lichrosphere RP-100 C8 column. The RSD was observed to 0.21 percentage and linearity range of (LOQ) 0.025 – 150 percentage of label claim established with 0.9999 correlation, 8 different brands marketed samples were successfully analysed for content uniformity and compared the results with the USP and other guidelines for acceptance criteria. The developed method was found precise, linear, rugged and robust for validated parameters. The method can be used for assay and the content uniformity determination of Rabeprazole Sodium in its tablet dosage form.
ABSTRACT
OBJECTIVE:To compare the in vitro dissolubility of four kinds of commercial chlorphenamine maleate tablets. METHODS: To determine the dissolubility of four kinds of domestic commercial chlorphenamine meleate tablets by paddle method and to analyse the dissolution parameters, T50, Td, m, by variance analysis method. RESULTS: The dissolution parame- ters of the different tablets were T50(30. 3 197, 17. 3 695, 20. 1038, l4. 3 651), Td(34. 6 088, 26. 7 162, 28. 0 514, 22. 1 593)and m (2. 7 676, 0. 8 505, 1. 0 992, 0. 8 448). CONCLUSION: The statistical results indicated that there were significant differences between them(P
ABSTRACT
OBJECTIVE:To establish a method for uncertainty analysis about the content of norethisterone and its content uniformity in HPLC determination of norethisterone tablets. METHODS: The mathematic model of uncertainty measurement was deduced in the procedure of determining the content and content uniformity in norethisterone tablets by HPLC, and the factors influencing the uncertainty were determined and the factors were evaluated. RESULTS: The combined uncertainty of both content and content uniformity were 1.2%; the extended uncertainty of both were 2.4%, and the determined content were (101.8?2.4)% and (102.3?2.4)% respectively. CONCLUSIONS: This method is applicable for the uncertainty analysis about the content and content uniformity of norethisterone tablets.