A new method for the determination of trace non-rare earth elements (NREEs) impurities in high-purity lanthanum oxide by HPLC combined with ICP-AES is proposed. The chromatographic retention behaviors of matrix (La) a...A new method for the determination of trace non-rare earth elements (NREEs) impurities in high-purity lanthanum oxide by HPLC combined with ICP-AES is proposed. The chromatographic retention behaviors of matrix (La) and NREEs were studied using 2-ethylhexyl hydrogen 2-ethylhexyl phosphonate (P507) chelating resin as the stationary phase and dilute nitric acid as the mobile phase. It is found that the use of pH 1.7 nitric acid enables effective elution of NREEs from HPLC column, but the lanthanum remains on the column. The experimental results show that a favorable separation between matrix lanthanum and NREEs can be obtained within 15 min. The method proposed is applied to the determination of 8 NREEs impurities in high-purity La2O3. The recoveries of 8 NREEs are in the range of 90 % similar to 110 %.展开更多
Alogliptin(AGLT),active ingredient of Alogliptin Benzoate(AGLT-BZ),is a new dipeptidyl peptidase-4(DPP-4)inhibitor for the treatment of type 2 diabetes.This study aimed to build a suitable method to determine the pote...Alogliptin(AGLT),active ingredient of Alogliptin Benzoate(AGLT-BZ),is a new dipeptidyl peptidase-4(DPP-4)inhibitor for the treatment of type 2 diabetes.This study aimed to build a suitable method to determine the potential related substances in AGLT-BZ bulk drug and tablets.Seven related substances in Alogliptin Benzoate substances were synthetized and identified by ^(1)H-NMR and ESI-MS.In addition,the impurities were detected by a gradient reverse-phase high performance liquid chromatography(RP-HPLC)with UV detection.The chromatographic system consisted of an Angilent Zobax SB-CN column(250×4.6 mm;5 μm).The mobile phase consisted of water/acetonitrile/trifluoroacetic acid 1900:100:1 v/v/v(solution A)and acetonitrile/water/trifluoroacetic acid 1900:100:1 v/v/v(solution B)using a gradient program at a flow rate of 1.0 ml/min with 278 nm detection and an injection volume of 20 ml.Additionally,selectivity,the limit of quantitation(LOQ)and limit of detection(LOD),linearity,accuracy,precision and robustness were determined.Linearity was good over the concentration range 50-1000 ng/ml and the coefficient of determination(R^(2))were 0.9991-0.9998.RSD% of the determination of precision were <2%(n=6).The method of RP-HPLC for the determination of impurities in AGLT-BZ was proved to be precise,accurate,robust and reliable.Three batches of self-made bulk drug and three dosages of commercial tablets were detected with this method.展开更多
A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was d...A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was developed using L1 column with gradient using the mobile phase consist of solvent-A (pH = 6.6, phosphate buffer + 0.5% Triethylamine) and solvent-B (90% Acetonitrile). The eluted compounds were monitored at 225 nm. Solifenacin Succinate & Tamsulosin Hydrochloride was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic stress conditions. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The limit of quantification results was ranged from 0.135 - 0.221 μg/mL for Solifenacin Succinate impurities and 0.043 - 0.090 μg/mL for Tamsulosin Hydrochloride impurities. This method is suitable for the estimation of impurities and assay of Solifenacin Succinate & Tamsulosin Hydrochloride in tablets dosage form.展开更多
A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The...A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The method was developed using L1 column (250 × 4.6 mm;5 μm) with gradient elution using the mobile phase consisting of solvent-A (0.1% Ortho phosphoric acid) and solvent-B (100% Acetonitrile);the gradient program (T<sub>min</sub>/%B) was set as 0/10, 5/10, 20/60, 40/60, 41/10 and 50/10. The eluted compounds were monitored at 265 nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The influence of Acid, Alkaline, Oxidative, Photolytic, Thermal and Humidity stress conditions, on drug product was studied. The limit of quantification results of Valsartan, Hydrochlorothiazide and their impurities are, VAL: 0.303 μg/mL, HCTZ: 0.019 μg/mL, VAL RC-B: 0.085 μg/mL, VAL RC-C: 0.327 μg/mL, HCT RC-A: 0.017 μg/mL, CTZ: 0.080 μg/mL and 5-Chloro HCT: 0.047 μg/mL. The proposed method is suitable for the estimation of Valsartan & Hydrochlorothiazide impurities in tablets dosage form.展开更多
目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定盐酸曲唑酮中相关杂质的含量。方法:采用Agilent ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm, 1.8μm),以0.1%甲酸溶液-乙腈为流动相,梯度洗脱,流速0.2 mL·min^(-1),...目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定盐酸曲唑酮中相关杂质的含量。方法:采用Agilent ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm, 1.8μm),以0.1%甲酸溶液-乙腈为流动相,梯度洗脱,流速0.2 mL·min^(-1),柱温30℃,采用电喷雾离子化源(ESI),多反应检测(MRM)模式,正离子模式扫描。结果:测定了盐酸曲唑酮原料药中的5个相关杂质,分别为三唑并吡啶酮、曲唑酮-N-氧化物、脱氯曲唑酮、4-乙基曲唑酮、曲唑酮异丁醚类似物,杂质在测定的质量浓度范围内线性关系良好,r均≥0.999 5;平均回收率为91.9%~99.4%,RSD≤3.9%;测定的3批原料药中均检出了曲唑酮N-氧化物和脱氯曲唑酮,其中2批还检测到极微量的4-乙基曲唑酮。结论:建立的方法可测定盐酸曲唑酮原料药中的5种相关杂质,能更有效的评估和控制其质量。展开更多
文摘A new method for the determination of trace non-rare earth elements (NREEs) impurities in high-purity lanthanum oxide by HPLC combined with ICP-AES is proposed. The chromatographic retention behaviors of matrix (La) and NREEs were studied using 2-ethylhexyl hydrogen 2-ethylhexyl phosphonate (P507) chelating resin as the stationary phase and dilute nitric acid as the mobile phase. It is found that the use of pH 1.7 nitric acid enables effective elution of NREEs from HPLC column, but the lanthanum remains on the column. The experimental results show that a favorable separation between matrix lanthanum and NREEs can be obtained within 15 min. The method proposed is applied to the determination of 8 NREEs impurities in high-purity La2O3. The recoveries of 8 NREEs are in the range of 90 % similar to 110 %.
文摘Alogliptin(AGLT),active ingredient of Alogliptin Benzoate(AGLT-BZ),is a new dipeptidyl peptidase-4(DPP-4)inhibitor for the treatment of type 2 diabetes.This study aimed to build a suitable method to determine the potential related substances in AGLT-BZ bulk drug and tablets.Seven related substances in Alogliptin Benzoate substances were synthetized and identified by ^(1)H-NMR and ESI-MS.In addition,the impurities were detected by a gradient reverse-phase high performance liquid chromatography(RP-HPLC)with UV detection.The chromatographic system consisted of an Angilent Zobax SB-CN column(250×4.6 mm;5 μm).The mobile phase consisted of water/acetonitrile/trifluoroacetic acid 1900:100:1 v/v/v(solution A)and acetonitrile/water/trifluoroacetic acid 1900:100:1 v/v/v(solution B)using a gradient program at a flow rate of 1.0 ml/min with 278 nm detection and an injection volume of 20 ml.Additionally,selectivity,the limit of quantitation(LOQ)and limit of detection(LOD),linearity,accuracy,precision and robustness were determined.Linearity was good over the concentration range 50-1000 ng/ml and the coefficient of determination(R^(2))were 0.9991-0.9998.RSD% of the determination of precision were <2%(n=6).The method of RP-HPLC for the determination of impurities in AGLT-BZ was proved to be precise,accurate,robust and reliable.Three batches of self-made bulk drug and three dosages of commercial tablets were detected with this method.
文摘A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was developed using L1 column with gradient using the mobile phase consist of solvent-A (pH = 6.6, phosphate buffer + 0.5% Triethylamine) and solvent-B (90% Acetonitrile). The eluted compounds were monitored at 225 nm. Solifenacin Succinate & Tamsulosin Hydrochloride was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic stress conditions. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The limit of quantification results was ranged from 0.135 - 0.221 μg/mL for Solifenacin Succinate impurities and 0.043 - 0.090 μg/mL for Tamsulosin Hydrochloride impurities. This method is suitable for the estimation of impurities and assay of Solifenacin Succinate & Tamsulosin Hydrochloride in tablets dosage form.
文摘A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The method was developed using L1 column (250 × 4.6 mm;5 μm) with gradient elution using the mobile phase consisting of solvent-A (0.1% Ortho phosphoric acid) and solvent-B (100% Acetonitrile);the gradient program (T<sub>min</sub>/%B) was set as 0/10, 5/10, 20/60, 40/60, 41/10 and 50/10. The eluted compounds were monitored at 265 nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The influence of Acid, Alkaline, Oxidative, Photolytic, Thermal and Humidity stress conditions, on drug product was studied. The limit of quantification results of Valsartan, Hydrochlorothiazide and their impurities are, VAL: 0.303 μg/mL, HCTZ: 0.019 μg/mL, VAL RC-B: 0.085 μg/mL, VAL RC-C: 0.327 μg/mL, HCT RC-A: 0.017 μg/mL, CTZ: 0.080 μg/mL and 5-Chloro HCT: 0.047 μg/mL. The proposed method is suitable for the estimation of Valsartan & Hydrochlorothiazide impurities in tablets dosage form.
文摘目的:建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定盐酸曲唑酮中相关杂质的含量。方法:采用Agilent ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm, 1.8μm),以0.1%甲酸溶液-乙腈为流动相,梯度洗脱,流速0.2 mL·min^(-1),柱温30℃,采用电喷雾离子化源(ESI),多反应检测(MRM)模式,正离子模式扫描。结果:测定了盐酸曲唑酮原料药中的5个相关杂质,分别为三唑并吡啶酮、曲唑酮-N-氧化物、脱氯曲唑酮、4-乙基曲唑酮、曲唑酮异丁醚类似物,杂质在测定的质量浓度范围内线性关系良好,r均≥0.999 5;平均回收率为91.9%~99.4%,RSD≤3.9%;测定的3批原料药中均检出了曲唑酮N-氧化物和脱氯曲唑酮,其中2批还检测到极微量的4-乙基曲唑酮。结论:建立的方法可测定盐酸曲唑酮原料药中的5种相关杂质,能更有效的评估和控制其质量。
