A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. ...A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.展开更多
A rapid, straightforward, sensitive, efficient, and cost-effective reverse-phase high-performance liquid chromatographic method was employed for the simultaneous determination of Sorbitol, Sodium Lactate, and Chloride...A rapid, straightforward, sensitive, efficient, and cost-effective reverse-phase high-performance liquid chromatographic method was employed for the simultaneous determination of Sorbitol, Sodium Lactate, and Chlorides in a drug solution for infusion. Sorbitol, Sodium lactate, and Chloride are all officially recognized in the USP monograph. Assay methods are provided through various techniques, with titrations being ineffective for trace-level quantification. Alternatively, IC, AAS, and ICP-MS, though highly accurate, are costly and often unavailable to most testing facilities. When considering methods, it’s important to prioritize both quality control requirements and user-friendly techniques. A simple HPLC simultaneous method was developed for the quantification of Chlorides, Sorbitol, and Sodium Lactate with a shorter run time. The separation utilized a Shimpack SCR-102(H) ion exclusion analytical column (7.9 mm × 300 mm, 7 μm), with a flow rate of 0.6 mL per min. The column compartment temperature was maintained at 40°C, and the injection volume was set at 10 μL, with detection at 200 nm. All measurements were conducted in a 0.1% solution of phosphoric acid. The analytical curves demonstrated linearity (r > 0.9999) in the concentration range of 0.79 to 3.8 mg per mL for Sodium Lactate (SL), 0.16 to 0.79 mg per mL for Sodium Chloride (SC), and 1.5 to 7.2 mg per mL for Sorbitol. Validation of the developed method followed the guidelines of the International Conference on Harmonization (ICH Q2B) and USP. The method exhibited precision, robustness, accuracy, and selectivity. In accelerated stability testing over 6 months, no significant variations were observed in organoleptic analysis and pH. Consequently, the developed method is deemed suitable for routine quality control analyses, enabling the simultaneous determination of Sodium Lactate, Sodium Chloride, and Sorbitol in pharmaceutical formulations and infusions.展开更多
Stability indicating RP-UPLC technique was developed for the simultaneous quantification of glycopyrrolate, methylparaben, and propylparaben in glycopyrrolate oral solution. The method was established by using gradien...Stability indicating RP-UPLC technique was developed for the simultaneous quantification of glycopyrrolate, methylparaben, and propylparaben in glycopyrrolate oral solution. The method was established by using gradient UPLC and a Waters Acquity UPLC BEH C18, 100 mm 2.1 mm, i.d 1.7 μm particle size column with a gradient program of mobile phase A and mobile phase B with a flow rate of 0.25 mL/minute, UV wavelength detection at 222 nm, column temperature of 40°C, injection volume of 2 μL, mobile phase A contains 0.05% trifluoro acetic acid in water and Acetonitrile (90:10) v/v and mobile phase-B contains 0.05% trifluoro acetic acid in water and Acetonitrile (10:90) v/v. The current research describes a single UPLC method for developing an assay method for Glycopyrrolate Oral solution that includes Glycopyrrolate (Active), Methylparaben (Preservative), and Propylparaben (Preservative). The assay method was validated in accordance with ICH guidelines. The retention times of glycopyrrolate, methyl paraben and propylparaben were 6.051 min, 3.458 min and 8.095 min, respectively. Linearity range of glycopyrrolate, methyl paraben and propylparaben were in the range of 4 - 32 μg per mL, 35 - 290 μg per mL and 4 - 32 μg per mL, respectively. Recovery of glycopyrrolate, methylparaben and propylparaben ranged from 100.1% to 98.9%, 100.2% - 100.8%, and 100.2% - 100.8%. Validation of analytical method demonstrated that the method is suitable, specific, linear, accurate, precise, rugged and stability indicating for estimating three components in the pharmaceutical dosage form.展开更多
For the quantitative determination of Fulvestrant, Benzyl alcohol, and Benzyl benzoate in Fulvestrant injection, an original RP-HPLC approach was developed. The gradient method was developed using HPLC and a Phenomene...For the quantitative determination of Fulvestrant, Benzyl alcohol, and Benzyl benzoate in Fulvestrant injection, an original RP-HPLC approach was developed. The gradient method was developed using HPLC and a Phenomenex Luna C8, 150 × 4.6 mm, i.d 3.0 μm particle size column with a gradient programme of mobile phases A and B. With a flow rate of 1.5 mL/minute, injection volume of 10 μL, and column temperature of 35°C, UV wavelength detection at 254 nm for Benzyl alcohol and Benzoyl Benzoate and 280 nm for Fulvestrant, mobile phase-A consists of DI water and mobile phase-B consists of Acetonitrile. The current study describes a single HPLC method for developing a Fulvestrant (Active), Benzyl alcohol (Cosolvent), and Benzyl Benzoate (Cosolvent) assay for Fulvestrant injection. The assay method was determined to be suitable for quantifying three components in the pharmaceutical product and was verified according to ICH guidelines.展开更多
文摘A novel, simple, and sensitive Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the quantification of process-related impurities and degradants, as well as the assay of Docetaxel. The stability-indicating capability of the method was demonstrated through forced degradation studies and a comprehensive mass balance evaluation. Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column (100 × 2.1 mm, 1.7 µm), with gradient elution. The mobile phase A comprised a mixture of water, methanol, and acetonitrile (500:300:200, v/v/v), while mobile phase B was acetonitrile and water (800:200, v/v). The flow rate was set at 0.4 mL/min, with detection at 232 nm using a photodiode array detector. The method exhibited excellent performance, with a tailing factor of 1.10 for Docetaxel. The method was rigorously validated for precision, accuracy, linearity, LOD, LOQ, ruggedness, specificity, and robustness. Forced degradation studies confirmed the method’s suitability for stability analysis. Stability testing on the drug substance was conducted following ICH guidelines.
文摘A rapid, straightforward, sensitive, efficient, and cost-effective reverse-phase high-performance liquid chromatographic method was employed for the simultaneous determination of Sorbitol, Sodium Lactate, and Chlorides in a drug solution for infusion. Sorbitol, Sodium lactate, and Chloride are all officially recognized in the USP monograph. Assay methods are provided through various techniques, with titrations being ineffective for trace-level quantification. Alternatively, IC, AAS, and ICP-MS, though highly accurate, are costly and often unavailable to most testing facilities. When considering methods, it’s important to prioritize both quality control requirements and user-friendly techniques. A simple HPLC simultaneous method was developed for the quantification of Chlorides, Sorbitol, and Sodium Lactate with a shorter run time. The separation utilized a Shimpack SCR-102(H) ion exclusion analytical column (7.9 mm × 300 mm, 7 μm), with a flow rate of 0.6 mL per min. The column compartment temperature was maintained at 40°C, and the injection volume was set at 10 μL, with detection at 200 nm. All measurements were conducted in a 0.1% solution of phosphoric acid. The analytical curves demonstrated linearity (r > 0.9999) in the concentration range of 0.79 to 3.8 mg per mL for Sodium Lactate (SL), 0.16 to 0.79 mg per mL for Sodium Chloride (SC), and 1.5 to 7.2 mg per mL for Sorbitol. Validation of the developed method followed the guidelines of the International Conference on Harmonization (ICH Q2B) and USP. The method exhibited precision, robustness, accuracy, and selectivity. In accelerated stability testing over 6 months, no significant variations were observed in organoleptic analysis and pH. Consequently, the developed method is deemed suitable for routine quality control analyses, enabling the simultaneous determination of Sodium Lactate, Sodium Chloride, and Sorbitol in pharmaceutical formulations and infusions.
文摘Stability indicating RP-UPLC technique was developed for the simultaneous quantification of glycopyrrolate, methylparaben, and propylparaben in glycopyrrolate oral solution. The method was established by using gradient UPLC and a Waters Acquity UPLC BEH C18, 100 mm 2.1 mm, i.d 1.7 μm particle size column with a gradient program of mobile phase A and mobile phase B with a flow rate of 0.25 mL/minute, UV wavelength detection at 222 nm, column temperature of 40°C, injection volume of 2 μL, mobile phase A contains 0.05% trifluoro acetic acid in water and Acetonitrile (90:10) v/v and mobile phase-B contains 0.05% trifluoro acetic acid in water and Acetonitrile (10:90) v/v. The current research describes a single UPLC method for developing an assay method for Glycopyrrolate Oral solution that includes Glycopyrrolate (Active), Methylparaben (Preservative), and Propylparaben (Preservative). The assay method was validated in accordance with ICH guidelines. The retention times of glycopyrrolate, methyl paraben and propylparaben were 6.051 min, 3.458 min and 8.095 min, respectively. Linearity range of glycopyrrolate, methyl paraben and propylparaben were in the range of 4 - 32 μg per mL, 35 - 290 μg per mL and 4 - 32 μg per mL, respectively. Recovery of glycopyrrolate, methylparaben and propylparaben ranged from 100.1% to 98.9%, 100.2% - 100.8%, and 100.2% - 100.8%. Validation of analytical method demonstrated that the method is suitable, specific, linear, accurate, precise, rugged and stability indicating for estimating three components in the pharmaceutical dosage form.
文摘For the quantitative determination of Fulvestrant, Benzyl alcohol, and Benzyl benzoate in Fulvestrant injection, an original RP-HPLC approach was developed. The gradient method was developed using HPLC and a Phenomenex Luna C8, 150 × 4.6 mm, i.d 3.0 μm particle size column with a gradient programme of mobile phases A and B. With a flow rate of 1.5 mL/minute, injection volume of 10 μL, and column temperature of 35°C, UV wavelength detection at 254 nm for Benzyl alcohol and Benzoyl Benzoate and 280 nm for Fulvestrant, mobile phase-A consists of DI water and mobile phase-B consists of Acetonitrile. The current study describes a single HPLC method for developing a Fulvestrant (Active), Benzyl alcohol (Cosolvent), and Benzyl Benzoate (Cosolvent) assay for Fulvestrant injection. The assay method was determined to be suitable for quantifying three components in the pharmaceutical product and was verified according to ICH guidelines.
