摘要
目的：建立同时测定比沙可啶原料药中二氯甲烷和乙酸乙酯残留量的方法。方法 ：采用顶空气相色谱法。色谱柱为以6%氰丙基苯基-94%二甲基聚硅氧烷（DB-624）为固定液的毛细管柱,程序升温,进样口温度为220℃,检测器为氢火焰离子化检测器,温度为250℃,载气为高纯氮气,载气流速为3.0 ml/min,分流比为1∶10,顶空加热温度为70℃,平衡时间为30 min,顶空瓶装样量为5 ml,顶空进样量为1 ml。结果：二氯甲烷和乙酸乙酯检测质量浓度线性范围分别为6-120μg/ml（r=0.999 9）、50-1 000μg/ml（r=0.999 9）;定量限分别为0.2、1.7μg,检测限分别为0.06、0.5μg;精密度、稳定性、重复性试验的RSD≤3%;加样回收率分别为100.30%-102.00%（RSD=0.63%,n=9）、100.10%-101.30%（RSD=0.44%,n=9）。结论：该方法操作简便、结果准确,可用于同时测定比沙可啶原料药中二氯甲烷和乙酸乙酯的残留量。
OBJECTIVE：To establish a method for simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material. METHODS：Head-space GC was performed on the capillary column of 6% cyanopropyl phenyl-94% dimethyl polysiloxane（DB-624）by temperature programming,the temperature of injector was 220 ℃,detector was flame ionization detector with temperature of 250 ℃,carrier gas was high purity nitrogen with the flow rate of 3.0 ml/min,split ration was 1 ∶ 10,headspace heating temperature was 70 ℃,equilibration time was 30 min,volume of headspace vial was 5 ml,and the injection volume was 1 ml. RESULTS：The linear range was 6-120 μg/ml for dichloromethane（r=0.999 9）and 50-1 000 μg/ml for ethyl acetate（r=0.999 9）;the limit of quantitation was 0.2,1.7 μg,limit of detection was 0.06,0.5 μg;RSDs of precision,stability and reproducibility tests were no higher than 3%;recoveries were 100.30%-102.00%（RSD=0.63%,n=9）and 100.10 %-101.30%（RSD=0.44%,n=9）. CONCLUSIONS：The method is simple and accurate,and can be used for the simultaneous residual determination of dichloromethane and ethyl acetate in bisacodyl raw material.
出处
《中国药房》
CAS
北大核心
2016年第30期4297-4299,共3页
China Pharmacy
