气相色谱电子捕获法测定盐酸氨基葡萄糖中一氯甲烷和一氯乙烷

Determination of Chloromethane and Chloroethane in D-Glucosamine Hydrochloride by Gas Chromatography Coupled with Electron Capture Detector

目的:建立测定盐酸氨基葡萄糖原料中一氯甲烷和一氯乙烷残留量的方法。方法:采用顶空气相色谱法。以二甲基亚砜(DMSO)为溶剂,检测器为电子捕获检测器(ECD),色谱柱为DB-5(30 m×0.530 mm×3.000 m)毛细管柱。进样温度:200℃,检测器温度:250℃,程序升温,载气为氮气,顶空瓶温度为45℃,平衡时间为40 min。结果:一氯甲烷和一氯乙烷达到基线分离,检测浓度分别在0.101~0.606μg·ml^(-1),0.129~0.774μg·ml^(-1)范围内线性关系良好(r分别为0.996 0、0.997 7),平均回收率分别为99.6%(RSD=5.0%,n=9)、98.5%(RSD=4.6%,n=9),定量限分别为0.055μg·ml^(-1),0.013μg·ml^(-1)。结论:本方法准确快速,可有效的分离、测定盐酸氨基葡萄糖原料中的微量一氯甲烷和一氯乙烷。

Objective： To establish a method for the determination of chloromethane and chloroethane in the raw material of D-glu- cosamine bydrochloride. Methods： Headspace gas chromatography was adopted. DMSO was taken as the solvent. The separation was performed on a DB-5 （30 m × 0. 530 mm × 3. 000 m）capillary column with ECD as the detector. The injection temperature was 200℃ , and the detector temperature was 250℃ with temperature programming. N2 was used as the carrier gas. The vial equilibration temperature was 45℃ with the equilibration time of 40 min. Results： The baseline resolution was achieved in the determination of chlorometh- ane and ehloroethane. The linear range was 0. 1014）. 606μg·ml^-1（ r = 0.996 0） and 0. 1294）. 774μg·ml^-1 with good linearity in the concentration （ r = 0. 997 7 ）, and the average recovery was 99.6% （ RSD = 5.0%, n = 9 ） and 98.5 % （ RSD = 4.6%, n = 9 ）, respectively. The limit of quantification was 0. 055 μg·ml^-1 and 0. 013μg·ml^-1 ,respectively. Conclusion： The method is accurate and rapid, and can be used for the effective separation and trace content determination of chloromethane and chloroethane in the raw material of bromhexine hydroehloride.