毛细管气相色谱法测定达格列净中7种有机溶剂的残留量

DETERMINATION OF RESIDUAL AMOUNT OF ORGANIC SOLVENTS IN DAPAGLIFLOZIN BY CAPILLARY COLUMN GAS CHROMATOGRAPHY

目的探讨达格列净中甲醇、乙醇、丙酮、异丙醇、乙腈、乙酸乙酯、四氢呋喃残留量的测定方法。方法采用毛细管气相色谱法,色谱柱为DB-624毛细管柱,程序升温,初始温度为40℃,保持10min,先以10℃/min的速率升温至80℃,再以70℃/min的速率升温至200℃,氢火焰离子化检测器(FID)。结果各组分能完全分离,甲醇、乙醇、丙酮、异丙醇、乙腈、乙酸乙酯和四氢呋喃的线性范围分别为0.0302~0.4824mg/ml(r=0.999 8)、0.0505~0.8078mg/ml(r=0.9999)、0.044~0.704 mg/ml(r=0.999 8)、0.0497~0.795 mg/ml(r=0.999 9)、0.0045~0.717mg/ml(r=0.998 5)、0.0502~0.803mg/ml(r=0.999 8)、0.0076~0.1216 mg/ml(r=0.9996);加样回收率为95.38%~100.89%。最低检测浓度为0.3、0.5、0.4、0.5、0.04、0.5、0.08μg/ml。结论该方法灵敏度和准确度均达到有机溶剂残留检测的要求,可用于达格列净中有机溶剂残留量的测定。

Objective To explore a method for the determination of residual amount of organic solvents in dapagliflozin. Methods Capillary gas chromatography was adopted with a DB-624 capillary column. The initial column temperature was 40℃, which was maintained for 10 minutes and then raised to 80~C by a rate of 10℃/min and then to 200℃ by a rate of 70 ℃/min. The flame ionization detector （FID） was used. Results Under the chromatographic condition, all solvents were separated thoroughly. The linear ranges of methanol, ethanol, acetone, isopropyl alcohol, acetonitrile, ethyl acetate and tetrahydrofuran were 0. 0302-0. 4824 mg/ml for methanol（ r =0. 999 8）, 0. 0505-0. 8078 mg/ml for ethanol（ r =0. 999 9）, 0. 044- 0. 704 mg/ml for acetone（ r =0. 999 8）, 0. 0497-0. 795 mg/ml for isopropanol（ r =0. 999 9）, 0. 0045-0. 717 rng/ml for acetonitrile（ r =0. 998 5）, 0. 0502-0. 803rag/m1 for ethanol acetate（ r =0. 999 8）and 0. 0076-0. 1216 mg/ml for tetrahydrofuran（ r =0. 999 6）respectively. The average recovery rate was between 95.38 %-100.89%. The lowest detection limits were 0. 3μg/ml, 0. 5μg/ml, 0. 4μg/ml, 0. 5μg/ml, 0. 04μg/ml, 0.5μg/ml and 0.08μg/ml respectively. Conclusion This is an accurate and sensitive method used for the detection of residual amount of organic solvents in dapagliflozin.