摘要:
目的 :采用顶空进样气相色谱法测定异丙基安替比林中残留甲醇、乙醇、丙酮的残留量。 方法 :使用配置顶空进样器的气相色谱仪,选择固定相为6％氰丙基苯基-94％二甲基聚硅氧烷、膜厚为3.0μm,0.53mm ×30m的色谱柱,以氮气为载气,顶空进样FID检测,通过外标法计算残留溶剂的含量。 结果 :异丙基安替比林中有乙醇检出。乙醇的线性范围:0.10-164.96μg／mL(r=0.999 9),甲醇的线性范围:0.21-164.72μg／ mL(r=0.999 9),丙酮的线性范围:0.10-163.36μg／mL(r=1.000 0);定量限乙醇、甲醇均为0.3μg／mL,丙酮为0.1μg／mL;平均回收率甲醇为101.0％(RSD=4.8％,n=6),乙醇为99.89％(RSD=4.4％,n=6),丙酮为99.85％(RSD=3.4％,n=6)。 结论 :本方法简便、灵敏度高、重复性好,结果准确,可用于异丙基安替比林原料药中有机溶剂残留量的测定。
Abstract:
Objective :To establish a method for determining residual solvents such as methanol,ethanol and acetone in propy-phenazone by headspace gas chromatography. Methods :The GC was equipped with a headspace injector and a flame-ionization dete(?) tor.A 0. 53mm×30m, DB-624 chromatographic column(coated with 6% cyanopropylphenyl-94% dimethyl polysiloxane) was adopted. The carrier gas was nitrogen.The assay of residual solvents were calculated according to the external standard method. Results :Only ethanol was found in the sample of propyphenazone.The standard curves were linear over the ranges of 0.10-164.96μg/mL(r= 0.9999) for ethanol,0.10-163. 36μg/mL(r=1.000 0) for acetone and 0.21-164.72μg/mL(r=0.999 9) for methanol. The limits of quantitation were 0. 3μg/mL for methanol and ethanol, 0. 1μg/mL for acetone.The average recoveries were 101. 0% ( RSD = 4.8% ,n=6)for methanol,99.89%(RSD=4.4%,n=6) for ethanol,99.85%(RSD=3.4%,n=6) for acetone. Conclusion :This method appeared to be sensitive,accurate,repeatable and easy to operate and was suitable for determining residual solvents of propyphenazone.
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