气相色谱法测定异丙基安替比林中的残留溶剂

Determination of residual solvents in propyphenazone by headspace GC

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。

Objective：To establish a method for determining residual solvents such as methanol , ethanol and acetone in propyphenazone by headspace gas chromatography. Methods ：The GC was equipped with a headspace injector and a flame -ionization detector. 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. 999 9） 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. Concluslon：This method appeared to be sensitive, accurate,repeatable and easy to operate and was suitable for determining residual solvents of pmpyphenazone.