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目的建立毛细管气相色谱法测定依折麦布中异丙醇、乙醇、二氯甲烷、乙酸乙酯、正庚烷、叔丁基甲基醚6种溶剂残留量。方法以Agilent DB-624毛细管柱(30 m×0.53 mm,3μm)为色谱柱,以氮气为载气,以氢火焰离子化检测器检测,以N,N-二甲基甲酰胺为溶剂,以乙腈为内标物,采用程序升温模式检测依折麦布原料药中异丙醇、乙醇、二氯甲烷、乙酸乙酯、正庚烷、叔丁基甲基醚的残留量。结果异丙醇、乙醇、二氯甲烷、乙酸乙酯、正庚烷、叔丁基甲基醚的定量限分别为0.63、0.63、2.40、0.75、0.50和0.50 mg·L-1;检测限质量浓度分别为0.32、0.32、1.20、0.38、0.25和0.25 mg·L-1。6种溶剂在线性范围内的相关系数均≥0.998 9,平均回收率均在98.7%~101.4%内。结论该方法可用于测定依折麦布中溶剂残留量。
OBJECTIVE To establish a capillary gas chromatographic method for the determination of 6 residual solvents of ezetimibe in isopropanol, ethanol, methylene chloride, ethyl acetate, n-heptane and tert-butyl methyl ether. Methods Agilent DB-624 capillary column (30 m × 0.53 mm, 3 μm) was used as the column. Nitrogen was used as a carrier gas and hydrogen flame ionization detector was used. N, N-dimethylformamide Acetonitrile was used as an internal standard. The temperature of the ezetimibe was used to detect the residues of isopropanol, ethanol, methylene chloride, ethyl acetate, n-heptane and tert-butyl methyl ether in the ezetimibe raw material. Results The limit of quantification of isopropanol, ethanol, methylene chloride, ethyl acetate, n-heptane and tert-butyl methyl ether were 0.63, 0.63, 2.40, 0.75, 0.50 and 0.50 mg · L -1, The correlation coefficient of 0.32,0.32,1.20,0.38,0.25 and 0.25 mg · L-1.6 solvents in the linear range were all ≥0.998 9, and the average recoveries were within 98.7% ~ 101.4%. Conclusion The method can be used to determine the ezetimibe solvent residues.