聚乳酸辅料中氯仿残留量的气固顶空色谱测定法

Determination of residual chloroform in the poly(L-lactic acid) with headspace solid-phase microextraction gas chromatography

目的 用气固顶空色谱法测定聚乳酸中氯仿的残留量。方法 研碎供试品 ,置针管中于 6 0℃保温进行气固顶空平衡 ,顶空气中的氯仿以气相色谱法测定 ,使用电子捕获检测器 ,SE 30为固定相 ,柱温为 4 0℃。结果 方法的精密度RSD为 3 4 % ,回收率为 96 6 % ,氯仿在 0～ 30 μg/L范围内线性良好 (r=0 9993) ,检出限为 0 2 3μg/L。 结论 为类似难溶性辅料的有机溶剂残留量检测提供了可靠的方法。

Objective To determine residual chloroform in poly(L-lactic acid) with headspace solid-phase microextraction gas chromatography.Methods The samples were pulverized and then put into injectors and were kept at 60℃ to achieve equilibrium between gas and solid phases. Chloroform in headspace gas-phase was determined by using gas chromatography with an electron capture detector, in which SE-30 was used as the stationary phase with a column temperature of 50 ℃.Results The RSD (relative standard deviation) of the method was 3.4% and the average recovery was 96.6%. The calibration curve remained linear within the chloroform concentration range of 0～30 μg/L(r=0.999 3)and the limit of detection was0.23 μg/L. Conclusion The method is more reliable for the determination of residual organic solvents in the similar hard-soluble accessories.