摘要
建立了气相色谱-质谱联用法（GC-MS）N定纺织品中1，2-二氯乙烷及其降解产物的方法。样品经甲醇超声提取后，降解物2．氯乙醇可直接用气质联用仪测定，氯乙酸经衍生为氯乙酸甲酯后，用气质联用仪测定，外标法定量。结果表明：在0．05～30mg／L范围内，1，2-二氯乙烷、2-氯乙醇、氯乙酸的线性相关系数分别为0．9996、0．9990、0．9990，在较宽的质量浓度范围内有很好的线性关系；方法的检测低限均为0．5mg／kg。7种阴性纺织品，在0．5、1．0和5．0mg／kg3个加标水平下，1，2-二氯乙烷、2-氯乙醇、氯乙酸的平均回收率范围为85．0％～101．6％，相对标准偏差为3．7％～7．9％。该方法简便、准确、灵敏度和精密度高，适用于纺织品中1，2-二氯乙烷及其降解产物的分析检测。
A gas chromatography-mass spectrometry （GC-MS） method is developed for determination of 1,2-dichloroethane and its degraded products in textiles. The samples are extracted with methanol un- der ultrasonic assistance. The separation and quantification of 1,2-dichloroethane and 2-chloroethanol are achieved by GC-MS. Chloroacetic acid is derived as methyl chloroacetate by esterification and then is detected by GC-MS. External standards are employed for the identification and quantification of ],2-di- chloroethane and its degraded products. The results indicate that the calibration curve shows good lin- ear relationship between peak area and concentration in the range of 0.05N30 mg/L with correlation coef- ficients of 0.999 6, 0.999 0 and 0.999 0 respectively. The limits of detection are 0.5 mg/kg. The average re- coveries of 1,2-dichloroethane, 2-chloroethanol and chloroacetic acid from 7 typical textile materials at three spiked concentration levels of 0.5 mg/kg, 1 mg/kg and 5 mg/kg are in the range of 85.0 % - 101.6 % with relative standard deviation （RSD） of 3.7% - 7.9 %. The method features low detection limit, good ac- curacy and high precision, and can be used for residue surveillance of 1,2-dichloroethane and its degrad- ed products in textile samples.
出处
《印染》
北大核心
2015年第1期39-43,共5页
China Dyeing and Finishing
关键词
测试
气相色谱法
质谱法
1
2-二氯乙烷
2-氯乙醇
氯乙酸
纺织品
testing
gas chromatography
mass spectrometry
1,2-dichloroethane
2-chloroethanol
chlo- roacetic acid
textiles
