顶空气相色谱法测定盐酸去甲万古霉素原料药中的10种有机溶剂残留量  

Determination of 10 Residual Organic Solvents in Norvancomycin Hydrochloride Raw Material by HS-GC

作　　者：耿文飞[1] 左明昊[1] 张晓楠[1] 唐蜜[1] 张雪霞[1] 佟杰[1] 

机构地区：[1]华北制药集团新药研究开发有限责任公司/微生物药物国家工程研究中心/河北省工业微生物代谢工程技术研究中心,石家庄050015

出　　处：《中国药房》2015年第21期2977-2979,共3页China Pharmacy

基　　金：国家科技重大专项子任务--重大新药创制(No.2014ZX09201001-004)

摘　　要：目的：建立测定盐酸去甲万古霉素原料药中10种有机溶剂残留量的方法。方法：采用顶空气相色谱方法。色谱柱为以硝基对苯二酸改性的聚乙二醇为固定液的DB-FFAP毛细管柱;初始温度为40℃,保持3 min,以8℃/min升温到150℃,保持10min;进样口温度为200℃;载气为高纯氮气,恒定流速为5 ml/min;分流比为15∶1;顶空瓶平衡温度为85℃,平衡时间为40 min;进样量为1 ml。结果：正戊烷、丙酮、乙醇、苯、丙烯腈、甲苯、二甲苯、氯苯、苯乙烯、二乙烯苯在各自质量浓度范围内与峰面积呈良好的线性关系（r为0.995 7~0.999 9）;精密度、重复性试验的RSD≤6.6%;回收率为94.3%~106.6%（RSD为0.5%~4.5%,n=9）。结论：该方法快速、灵敏、准确,可用于盐酸去甲万古霉素原料药中有机溶剂残留量的测定。OBJECTIVE：To establish the method for determining 10 residual organic solvents in norvancomycin hydrochloride raw material. METHODS：Headspace gas chromatography was performed on the column of nitro modified polyethylene terephthalate glycol as stationary phase capillary column;the oven temperature program started at 40 ℃ for 3 min and increased at a rate of8 ℃/min up to 150 ℃ for 10 min;the temperature was 200 ℃ with carrier gas of high-purity nitrogen gas,the constant flow rate was 5 ml/min with split ratio of 15 ∶ 1;the headspace vial equilibrium temperature was 85 ℃ with equilibrium time of 40 min,and the volume was 1 ml. RESULTS：The concentration of n-pentane,acetone,ethanol,benzene,acrylonitrile,toluene,xylene,chlorobenzene,styrene,divinylbenzene had good linear relationship with its peak area values（r=0.995 7-0.999 9）;the RSDs of precision,repeatability tests was ≤6.6%;average recovery was in the range of 94.3%-106.6%（RSD=0.5%-4.5%,n=9）. CONCLUSIONS：The method is fast,sensitive and accurate,and can be used for the determination of residual organic solvents in norvancomycin hydrochloride raw material.

关 键 词：盐酸去甲万古霉素 大孔树脂 残留溶剂 顶空气相色谱法 

分 类 号：R917[医药卫生—药物分析学]