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目的建立测定薁磺酸钠原料药中1,2-二氯乙烷和1,4-二氧六环两种有机溶剂残留量的方法。方法采用二甲基亚砜为顶空溶剂的毛细管顶空气相色谱法。结果1,2-二氯乙烷和1,4-二氧六环的线性范围分别为0.03~0.50μg·mL-1、2.38~38.0μg·mL-1(r分别为0.9995、0.9999),平均回收率分别为95.6%、97.2%,RSD分别为2.0%、1.5%(n=5)。结论所建方法快速简便、准确可靠,适合薁磺酸钠原料药中有机溶剂残留量的测定。
Objective To establish a method for the determination of the residues of 1,2-dichloroethane and 1,4-dioxane in organic sodium sulfonate raw materials. Methods Capillary headspace gas chromatography with dimethylsulfoxide as a headspace solvent. Results The linear ranges of 1,2-dichloroethane and 1,4-dioxane were 0.03 ~ 0.50μg · mL-1 and 2.38 ~ 38.0μg · mL-1 respectively (r = 0.9995,0.9999, respectively) The recoveries were 95.6% and 97.2%, respectively, with RSDs of 2.0% and 1.5%, respectively (n = 5). Conclusion The proposed method is rapid, simple, accurate and reliable and suitable for the determination of organic solvents in sodium sulfonate raw materials.