顶空气相色谱法同时测定比沙可啶原料药中2种溶剂残留量 点击下载
论文标题: 顶空气相色谱法同时测定比沙可啶原料药中2种溶剂残留量
英文标题:
中文摘要: 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6~120 μg/ml(r=0.999 9)、50~1 000 μg/ml(r=0.999 9);定量限分别为0.2、1.7 μg,检测限分别为0.06 、0.5 μg;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。
英文摘要: 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.
期刊: 2016年第27卷第30期
作者: 姜建国,孙婷,郭永辉,韩学静,苗会娟
英文作者: JIANG Jianguo,SUN Ting,GUO Yonghui,HAN Xuejing,MIAO Huijuan
关键字: 比沙可啶;顶空气相色谱法;溶剂残留量;二氯甲烷;乙酸乙酯
KEYWORDS: Bisacodyl; Head-space GC; Residual determination; Dichloromethane; Ethyl acetate
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