气相色谱法测定阿奇霉素原料中的溶媒残留量

Determination of Residual Solvents in Azithromycin Raw Material by GC

目的建立以气相色谱法测定阿奇霉素原料中残留溶媒二氯甲烷、丙酮和乙醇含量的方法。方法色谱柱为玻璃柱,进样温度为140℃,柱温为160℃,载气为氮气,柱前压为30Psi,并以氢火焰离子化检测器进行检测。结果二氯甲烷、丙酮、乙醇检测浓度分别在0·02%～0·1%(r=0·9995)、0·05%～0·25%(r=0·9994)、0·02%～0·1%(r=0·9994)范围内线性关系良好;平均回收率分别为99·1%(RSD=1·4%)、100·1%(RSD=1·1%)、99·5%(RSD=1·3%)。3批阿奇霉素原料中有机溶媒残留量均符合规定。结论本方法灵敏、准确、可靠,可用于本品有机溶媒残留量的测定。

OBJECTIVE：To determine the contents of the residual solvents including dichloromethane,acetone and ethanol in azithromyein raw material by GC.METHODS： A glass column was used as chromatographic column.The temperature of sample injection was 140℃ and column temperature was 160℃ .The carrier gas was nitrogen.The column inlet pressure was 30Psi.The detection was performed using hydrogen flame ionization detector.RESULTS： The detection concentrations of dichloromethane, acetone and ethanol were 0.02%-0.1% （r = 0.9 995）, 0.05% -0.25% （r = 0.9 994） and 0.02% -0.1% （r = 0.9 994）, respectively.The average recovery were 99.1% （RSD- 1.4%）, 100.1% （RSD- 1.1%） and 99.5% （RSD- 1.3%）, respectively.All of the three batches of samples were up to the standard with regard to the residual volume of organic solvent residues in azithromycin raw material.CONCLUSION：The method is proved to be accurate, sensitive and reliable, and suitable for the detection of organic solvent residues in azithromycin.