| Chial drugs are widely favored by the doctors and patients as they have high assay,good curative effect and less Adverse Drug Reaction.HPLC Chiral Stationary Phase is one of the mature methods,due to its high separation performance and simplicity,and is widely used.HPLC methods for determine of the chiral impurities of Dex-ketoprofen Trometamol and Atomoxetine HCl together with the intermediate N-Methyl Paroxetine were established based on the resolution performance.The resolution performance was obtained based on comparison of the results from different columns,mobile phase solvent composition and flow rate and also the column temperature.Analytical method was established and validated,the results were as follow:1.The final method conditions employing a DAICEL OJ-RH column and mobile phase of n-hexane/isopropanol/acetic acid(9:1:0.03)at 1.0 mL/min under the column at 30? were established for analysis of chiral impurity in Dex-ketoprofen Trometamol.The quantitation limit was 0.243 ?g/mL,the response of the impurity was linear(R~2=1)in the concentration range of 0.243~30.3 ?g/mL.The recovery was 92.8~115.7% and RSD for precision was 3.6%.2.The final method conditions employing a CHIRALCEL OD-H column and mobile phase of n-hexane/isopropanol/diethylamine(85:15:0.2)at 1.0 mL/min under the column at 30? were established for analysis of chiral impurity in Atomoxetine HCl.The quantitation limit was 1 ?g/mL,the response of the impurity was linear(R~2=0.9983)in the concentration range of 0.90~1.5?g/mL.The recovery was 86.3~112.8% and RSD for precision was 0.9%.3.The final method conditions employing a CHIRALPAK AD-H column and mobile phase of n-hexane/ethanol/water/trifluoroacetic acid(900:105:2:1.95)at 1.0 mL/min under the column at 25? were established.The quantitation limit was 2.5 ?g/mL,the response of the impurity was linear(R~2=0.9909)in the concentration range of 2.5 ~38 ?g/mL.The recovery was 109.5~115.6% and RSD for precision was 0.8%. |
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