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目的建立顶空毛细管柱气相色谱法测定帕利哌酮中的溶剂残留量。方法以Agilent DB-624(30 m×530μm,3μm)柱为色谱柱,以氮气为载气,以氢火焰离子化检测器检测,以N,N-二甲基乙酰胺为溶剂,采用程序升温模式检测帕利哌酮原料药中甲醇、乙酸乙酯、二氯甲烷和三乙胺的残留量。结果 4种挥发性有机溶剂均达到基线分离,在考察的质量浓度内线性良好(r≥0.999 0),平均回收率分别为103.1%、101.9%、101.3%和100.8%,RSD分别为2.9%、2.8%、3.3%和6.2%(n=9)。结论该方法操作简单、快速、灵敏、可靠,可用于帕利哌酮原料药中4种有机溶剂残留量测定。
Objective To establish a headspace capillary gas chromatographic method for the determination of residual solvents in paliperidone. Methods Agilent DB-624 column (30 m × 530 μm, 3 μm) was used as the column. Nitrogen gas was used as a carrier gas and detected by hydrogen flame ionization detector. N, N-dimethylacetamide The mode was to determine the residues of methanol, ethyl acetate, methylene chloride and triethylamine in Paliperidone APIs. Results The four volatile organic solvents all achieved baseline separation with good linearity (r≥0.999 0) and mean recovery rates of 103.1%, 101.9%, 101.3% and 100.8%, respectively, with RSDs of 2.9% 2.8%, 3.3% and 6.2% (n = 9). Conclusion The method is simple, rapid, sensitive and reliable. It can be used for the determination of four organic solvents residues in raw materials of Paliperidone.