Determination of Six Organic Solvent Residues in Active Pharmaceutical Ingredients of Dydrogesterone Drug by HS-GC
Objective:To establish a gas chromatography to measuring residual solvents in dydrogesterone drug substance.Methods:The capillary column with 6％cyanopropyl phenyl-94％dimethylpolysiloxane as fixative is chromatography column(DB-624,30 mx0.53 mm,film thickness 3.00 μm),the procedure heating,temperature of flame ionization detector is 240 ℃,inlet temperature is 200 ℃,carrier gas is nitrogen,flow rate is 2 mL/min,shunt ratio is 10:1,top space injection sample is 1 μL.Results:The quantitative limit concentrations of ethanol,acetone,N-hexane,dichloromethane,ethyl acetate and isopropanether were 5.222 0,5.362 0,0.592 9,0.294 2,5.184 0,5.242 0 μg·mL-1,respectively,Detection limit concentrations were 1.566 6,1.608 6,0.177 9,0.088 3,1.555 2,1.572 6 μg·ml-1,respectively,Have a good linearity in the measured concentration range,The correlation coefficient(r)is greater than 0.990,The average recovery rates were 105.06％,102.02％,106.78％,100.13％,100.99％and 103.06％,respectively.Conclusion:The detection method is easy to operate and suitable to detect the residual amount of 6 residual solvents in dydrogesterone.
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