Gradient high performance liquid chromatography method for simultaneous determination of ilaprazole and its related impurities in commercial tablets

A methodology(HPLC)proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated.The chromatographic separation was carried out by gradient elution using an Agilent C8 column(4.6 mm×250 mm,5 mm)which was maintained at 25℃.The mobile phase composed of solvent A(methanol)and solvent B(solution consisting 0.02 mmol/l monopotassium phosphate and 0.025 mmol/l sodium hydroxide)was at a flow rate of 1.0 ml/min.The samples were detected and quantified at 237 nm using an ultraviolet absorbance detector.Calibration curves of all analytes from 0.5 to 3.5 mg/ml were good linearity(r≥0.9990)and recovery was greater than 99.5% for each analyte.The lower limit of detection(LLOD)and quantification(LOQ)of this analytical method were 10 ng/ml and 25 ng/ml for all impurities,respectively.The stress studies indicated that the degradation products could not interfere with the detection of ilaprazole and its related impurities and the assay can thus be considered stability-indicating.The method precisions were in the range of 0.41-1.21 while the instrument precisions were in the range of 0.38-0.95 in terms of peak area RSD% for all impurities,respectively.This method is considered stabilityindicating and is applicable for accurate and simultaneous measuring of the ilaprazole and its related impurities in commercial enteric-coated tablets.

Simultaneous Analysis of Indapamide and Related Impurities in Sustained-Release Tablets by a Single-Run HPLC-PDA Method

The contents of indapamide and related impurities in generic indapamide sustained-release tablets were simultaneously detected by a single-run high performance liquid chromatography equipped with photodiode array detector(HPLC-PDA)method for the quality control in this paper.The results showed the method had a good selectivity and was validated through linearity,limits of detection and quantification,recovery,and precision.The linear ranges of indapamide,2-methyl-1-nitroso-2,3-dihydro-1H-indole(impurity A,ImA),4-chloro-N-(2-methyl-1H-indol-1-yl)-3-sulphamoyl-benzamide(impurity B,ImB)and 4-chloro-3-sulfamoylbenzoic acid(impurity 1,Im1)were 0.028-1.80μg/mL(R=0.99995),0.060-1.20μg/mL(R=0.9996),0.0324-1.20μg/mL(R=0.99985)and 0.060-1.20μg/mL(R=0.9997)with detection limits of 0.0093,0.012,0.012 and 0.006μg/mL,respectively.ImA and Im1 were not detectable in the generic drug.The content of indapamide was 96.7%of the labeled amount with a relative standard deviation(RSD)of 1.30%,and the percentage of ImB relative to the labeled amounts of indapamide was 0.106%with an RSD of 1.82%.The content of other unspecified impurities all met the reference quality standards.The results provided references for the quality control and the quality standard study of generic indapamide sustained-release tablets.

Morphological and Microstructural Evolution and Related Impurity Incorporation in Non-Polar a-Plane GaN Grown on r-Sapphire Substrates

Effects of the growth temperature on morphological and microstructural evolution of a-plane GaN films grown on r-plane sapphires by metal organic chemical vapor deposition are investigated by atomic force microscopy and secondary ion mass spectroscopy （SIMS）. Surface morphology, structural quality and related impurity incorpora- tion are very sensitive to the growth temperature. A significant difference of yellow luminescence is observed and attributed to the incorporation of carbon into GaN films, which is confirmed by SIMS analysis. Our results show that the sample with triangular-pit morphology has sample with pentagon-like pit morphology, which is significantly higher concentrations of oxygen than the other induced by the existence of an N-face in triangular pits.

LC–UV/MS quality analytics of paediatricartemether formulations

A highly selective and stability-indicating HPLC-method, combined with appropriate sample preparation steps, is developed for β-artemether assay and profiling of related impurities, including possible degradants, in a complex powder for oral suspension. Following HPLC conditions allowed the required selectivity： a Prevail organic acid （OA） column （250 mm＆#215;4.6 mm, 5μm）, flow rate set at 1.5 mL/min combined with a linear gradient （where A ？ 25 mM phosphate buffer （pH 2.5）, and B ？ acetonitrile） from 30% to 75% B in a runtime of 60 min. Quantitative UV-detection was performed at 210 nm. Acetonitrile was applied as extraction solvent for sample preparation. Using acetonitrile-water mixtures as extraction solvent, a compartmental behaviour by a non-solving excipient-bound fraction and an artemether-solubilising free fraction of solvent was demonstrated, making a mobile phase based extraction not a good choice. Method validation showed that the developed HPLC-method is considered to be suitable for its intended regulatory stability-quality characterisation of β-artemether paediatric formulations. Furthermore, LC-MS on references as well as on stability samples was performed allowing identity confirmation of the β-artemether related impurities. MS-fragmentation scheme of β-artemether and its related substances is proposed, explaining the m/z values of the in-source fragments obtained.

Deep Purification of Zinc Ammoniacal Leaching Solution by Cementation with Zinc Dust

Deep purification of zinc ammoniacal leaching solution by cementation using zinc dust was studied.The effects of relative amount of metallic impurities,dosage of zinc dust,purification time,temperature,pH value and total ammonia concentration in the solution on the purification of the solution were investigated.The results indicate that total ammonia concentration in the solution had no effect on the purification,but relative amount of metallic impurities,dosage of zinc dust,purification time,temperature and pH value of the solution were the main factors influencing the purification.Keeping appropriate molar ratio of copper to cadmium or nickel to cadmium was beneficial to the cementation of cadmium.Nevertheless,the presence of cobalt went against the cementation of cadmium and cobalt.All metallic impurities could be decreased to acceptable levels under the optimized conditions of 2 g/L of zinc dust dosage,1 h of purification time,35℃,pH value 9.03 of zinc ammoniacal leaching solution.The deeply purified zinc ammoniacal solution obtained by one-stage purification meets the requirements of zinc electrowinning.