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顶空气相色谱法同时测定某原料药中8种有机残留溶剂方法

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目的 建立了同时测定某原料药中甲醇、乙醇、异丙醇、二氯甲烷、四氢呋喃、2-甲基四氢呋喃、醋酸异丙酯、N,N-二甲基甲酰胺8种有机溶剂残留量的顶空气相色谱法。方法 采用顶空气相色谱法,色谱柱为CP-Volamine毛细管柱(30 m×0。32 mm);载气为氮气,程序升温:起始温度为40 ℃,保持5 min,以20 ℃·min-1升温至220 ℃,保持5 min;顶空平衡温度为100 ℃,平衡时间15 min。结果 8种有机残留溶剂均完全分离;各对照品均在各自的质量浓度范围内与峰面积线性关系良好;8种有机残留溶剂的回收率为99。3%~103。6%,RSD为1。7%~4。9%(n=6)。两种进样方式对N,N二甲基甲酰胺含量检测无显著差异。结论 该方法操作简便、结果准确、重复性好,可用于同时测定某原料药中8种有机溶剂的残留量。
Detection Method for Eight Residual Solvents in Raw Materials with Headspace Gas Chromatography
Objective To establish a headspace gas chromatography method for the determination of methanol,ethanol,isopropanol,dichloromethane,tetrahydrofuran,2-methyltetrahydrofuran,isopropylace-tate and N,N-dimethylformamide.Methods A headspace gas chromatography method was used to separate the residual solvents on a CP-Volamine capillary column(30 m×0.32 mm).The carrier gas was nitrogen.The initial temperature of the column was 40 ℃ for 5 min and was raised to 220 ℃ at the rate of 20 ℃·min-1 for 5 min.The equilibrium temperature of the headspace injector was 100 ℃ that lasted for 15 min.Results The eight solvents were well separated.The linearity was good within their respective concentra-tion ranges.The recovery ranged from 99.3%to 103.6%,with an RSD of 1.7%-4.9%(n=6).There was no significant difference in the detection of formamide content between the two injection methods.Conclusion The established method is sensitive and accurate,and suitable for the determination of residual solvents in raw materials.

headspace gas chromatographyresidual solventsraw materials

余小翠、王习文、高锦、赵莹莹、祝雨薇、胡丹

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100166 北京,联勤保障部队药品仪器监督检验总站

顶空气相色谱法 残留溶剂 原料药

2024

解放军药学学报
中国人民解放军总后勤部卫生部 药品仪器检验所

解放军药学学报

影响因子:0.529
ISSN:1008-9926
年,卷(期):2024.37(4)