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Forced degradation studies of gliquidone were conducted under different stress conditions. Three degradates were observed upon using HPLC and TLC and elucidated by LC-MS and IR. HPLC method was performed on C18 column using methanol-water (85:15 v/v) pH 3.5 as a mobile phase with isocratic mode at 1 mL.min-1 and detection at 225 nm. HPLC analysis was applied in range of 0.5-20 µg.mL-1 (r =1) with limit of detection (LOD) 0.177 µg.mL-1. TLC method was based on the separation of gliquidone from degradation products on silica gel TLC F254 plates using chloroform-cyclohexane-glacial acetic acid (6:3:1v/v) as a developing system with relative retardation 1.15±0.01. Densitometric measurements were achieved in range of 2 -20 µg /band at 254 nm (r = 0.9999) with LOD of 0.26 µg /band. Least squares regression analysis was applied to provide mathematical estimates of the degree of linearity. The analysis revealed a linear calibration for HPLC where a binomial relationship for TLC. Stability testing and methods validation have been evaluated according to International Conference on Harmonization guidelines. Moreover, the proposed methods were applied for the analysis of tablets and the results obtained were statistically compared with those of pharmacopeial method revealing no significant difference about accuracy and precision.
Subject(s)
Chromatography, High Pressure Liquid/methods , Hypoglycemic Agents/metabolism , Densitometry/methods , Diabetes Mellitus, Type 2/drug therapy , Drug StabilityABSTRACT
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.
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Objective:To develop a simple and rapid HPLC method to determine the concentration and pharmacokinetics of gliqui-done in human plasma. Methods: Acetonitrile was used to precipitate plasma proteins directly and gliquidone was detected by an HPLC-fluorescence assay. The mobile phase consisted of acetonitrile-20 mmol·L-1 biphosphate potassium (80∶20, v/v, pH 2. 5). The flow rate was 1. 0 ml·min-1 . The excitation wavelength was 315 nm and the emission wavelength was 410 nm. Results:The line-arity of gliquidone in plasma was good from 0. 034 to 2. 2 μg·ml-1 and the quantitative lower limit was 0. 034 μg·ml-1 . The range of method recovery was 99. 23%-108. 11%, and that of extraction recovery was 85. 78%-88. 77%. The intra-and inter-day precision was both less than 10%. Both specificity and stability met the requirements. Gliquidone in plasma was determined using the above method after a single oral dose of 60 mg gliquidone tablets in 20 healthy volunteers, and then the pharmacokinetic parameters were ana-lyzed. The variation coefficients were close to or more than 50%. Conclusion:The method is simple, rapid and sensitive, and suit-able for the detection of gliquidone in a large quantity. Individualized administration of gliquidone should be considered due to the obvi-ous individual difference in pharmacokinetics.
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Objective To investigate the effects of gliquidone on the AGEs (advanced glycation end products) -induced RANTES(Regulated upon activation,normal T-cell expressed and secreted) expression of human renal mesangial cells (HRMC). Methods AGEs were prepared by incubation of bovine serum albumin (BSA) with high concentration of glucose at 37℃ in vitro. HRMC was cultured in the presence of AGE-BSA (glucose at 50 mmol/L) with or without gliquidone. RANTES mRNA was analyzed by semi-quantity RT-PCR. The concentration of RANTES in the supernatant was quantified by ELISA. Results Gliquidone significantly inhibited the expression and secretion of RANTES induced by AGE-BSA. The inhibition of RANTES expression and secretion was in dose and time dependent manners. Conclusions AGEs is a potential toxin to induce expression of RANTES in HRMCs, which is inhibited by gliquidone.
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Objective To investigate the effects of gliquidone on the AGEs (advanced glycation end products) -induced RANTES(Regulated upon activation,normal T-cell expressed and secreted) expression of human renal mesangial cells (HRMC). Methods AGEs were prepared by incubation of bovine serum albumin (BSA) with high concentration of glucose at 37℃ in vitro. HRMC was cultured in the presence of AGE-BSA (glucose at 50 mmol/L) with or without gliquidone. RANTES mRNA was analyzed by semi-quantity RT-PCR. The concentration of RANTES in the supernatant was quantified by ELISA. Results Gliquidone significantly inhibited the expression and secretion of RANTES induced by AGE-BSA. The inhibition of RANTES expression and secretion was in dose and time dependent manners. Conclusions AGEs is a potential toxin to induce expression of RANTES in HRMCs, which is inhibited by gliquidone
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OBJECTIVE: To prepare gliquidone solid dispersion and to investigate its dissolution rate. METHODS: The gliquidone solid dispersion was prepared by dissolvent- fusion method and dissolvent method with PEG- 6000( PEG) and PVP K30( PVP) as carriers. RESULTS: The results of in vitro dissolubility test showed that the higher the carrier ratio, the faster the drug dissolution. The in vitro dissolubility of solid dispersions was faster with PVP than with PEG as carrier. The dissolution rate of the gliquidone- PVP ( 1∶ 7) solid dispersion reached as high as above 70% in 10 minutes, which was superior to that of its bulk drug. CONCLUSION: The gliquidone solid dispersion has been prepared successfully.
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0.05) among these pharmacokinetic parameters. The relative bioavailability of the test preparation was(107.8?30.0)%. CONCLUSION: The test and the reference preparation are bioequivalent.
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Objective To observe the clinical effect of Qushi Hua yu Tongluo Formu la (Prescriptions for dissolving damp, removing stasis, and eliminating obstruct ion of meridians) on hyperuricemia complicated with diabetes. Methods Totally 60 patients were randomized into a treatment group and a control gr oup with 30 in each. The control group was administered Gliquidone 30mg, three t imes a day, while the treatment group was added Qushi Huayu Tongluo F ormula, one dosage per day. Both groups were treated for 90 days. The clinical e ffect and the changes in serum uric acid, renal functions, blood lipid, and gly cosylated hemoglobin of both groups were observed. Results The total effective rate of the treatment groups and control groups was 93.34% and 23.33% respectiv ely, the difference was significant (P