顶空气相色谱法检测他达拉非原料药中4种溶剂残留量

目的建立测定他达拉非原料药中4种常见溶剂(甲醇、乙腈、异丙醇、四氢呋喃)残留量的顶空气相色谱法。方法采用顶空进样方式,分离柱采用DB-624柱(30 m×0.53 mm,3.0μm),程序升温,进样口温度为230℃,分流比为5∶1,载气为高纯氮气(纯度为99.999%),载气流速为1.8 mL/min;采用氢火焰离子化检测器检测,检测器温度为250℃。外标法定量。结果甲醇、乙腈、异丙醇、四氢呋喃的质量浓度线性范围分别为0.66~1.5 mg/mL,0.0082~0.205 mg/mL,0.06~1.5 mg/mL,0.0144~0.36 mg/mL;平均加样回收率分别为101.22%,100.59%,97.74%,100.73%,RSD分别为4.67%,2.63%,1.01%,2.28%(n=6);检测限分别为2μg/mL,8μg/mL,5μg/mL,6μg/mL。结论该方法操作简单,灵敏度高,准确性好,为可他达拉非中有机溶剂残留量的控制提供依据。

Determination of Four Residual Solutions in the Bulk Drug of Tadalafil by Headspace GC

Objective To develop a method for the determination for 4 residual solutions methanol,acetonitrile,isopropanol,and tetrahydrofuran(THF)in the bulk drug of tadalafil by headspace gas chromatography(GC)method.Methods Headspace injection mode was adopted and DB-624 column(30 m×0.53 mm,3.0μm)was selected as separation column.The injecting port temperature was 230℃with shunting ratio 5∶1;nitrogen(purity:99.999%)was used as carrier gas with flowing rate of 1.8 mL/min;hydrogen flameionization detector(FID)was used for detection with detector temperature of 250℃.External standard method was used for quantitative.Results The calibration curve of methanol,acetonitrile,isopropanol and THF showed good linear relationship within the ranges of 0.66-1.5,0.0082-0.205,0.06-1.5 and 0.0144-0.36 mg/mL.The average recoveries were 101.22%,100.59%,97.74%,100.73%,and the RSDs were 4.67%,2.63%,1.01%,2.28%,respectively(n=6).The detection limit was 2μg/mL for methanol,8μg/mL for acetonitrile,5μg/mL for isopropanol,and 6μg/mL for THF.Conclusion The method is simple,sensitive with good reproducible results,which can be applied to the quality control of residues in tadalafil.