论文部分内容阅读
目的建立血中1,2-二氯乙烷(1,2-DCE)的气相色谱-质谱测定方法。方法采用静态顶空分析法,血样中的1,2-DCE经DB-5MS弹性毛细管色谱柱分离,采用气相色谱-质谱联用仪检测,选择离子定量用62.0质荷比(m/z),确认用49.0、98.0 m/z,测定血样中1,2-DCE。结果血样中1,2-DCE在0.63~93.98μg/L线性关系良好,相关系数为0.999 7,定量下限为0.63μg/L(取血样2.0 ml)。批内相对标准偏差(RSD)为2.9%~6.7%,批间RSD为3.4%~8.1%,加标回收率为83.2%~94.1%,样品在-8℃以下可保存7 d。结论本法灵敏度高、干扰少、精密度和准确度好、操作简便,可作为检测职业中毒患者血中1,2-DCE的方法。
Objective To establish a method for the determination of 1,2-dichloroethane (1,2-DCE) in blood by gas chromatography-mass spectrometry. Methods The static headspace analysis method was used. The 1,2-DCE in blood samples was separated by capillary column chromatography (DB-5MS) and detected by gas chromatography-mass spectrometry (GC-MS) It was confirmed that blood 1,2-DCE was measured at 49.0 and 98.0 m / z. Results The linearity of 1,2-DCE in blood samples was 0.63 ~ 93.98μg / L with a correlation coefficient of 0.999 7 and a lower limit of quantitation of 0.63μg / L (blood sample 2.0ml). The relative standard deviations (RSDs) in batches ranged from 2.9% to 6.7%. The inter-batch RSD ranged from 3.4% to 8.1%. The spiked recoveries ranged from 83.2% to 94.1%. The samples were stored below -8 ° C for 7 days. Conclusion This method has high sensitivity, less interference, good precision and accuracy, easy operation, as a method to detect 1,2-DCE in blood of patients with occupational poisoning.