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目的建立血清中氯乙酸应急检测方法。方法血清中氯乙酸用甲基叔丁基醚萃取,用质量分数为10%硫酸/甲醇溶液衍生,气相色谱-电子俘获检测器(GC-ECD)测定。结果血清中氯乙酸低(200μg/L)?高(1000μg/L)2个质量浓度的加标回收率分别为85.6%?91.5%,批内精密度分别为3.9%、3.3%,批间精密度为9.7%～8.1%;该法在0～6.2mg/L范围内具有良好的线性关系,相关系数0.9999;最低定量下限为30μg/L,最低检出质量浓度为10μg/L(以1ml血清计),血样在4℃冷藏可以保存1周,在-20℃可保存2周。结论该法各项技术指标符合GBZ/T210.5—2008研制规范要求,可用于检测职业中毒人群血清中的氯乙酸水平。
Objective To establish a method of serum chloroacetic acid emergency detection. Methods Serum chloroacetic acid was extracted with methyl tert-butyl ether and derivatized with 10% sulfuric acid / methanol solution. Gas chromatography-electron capture detector (GC-ECD) was used to determine the concentration of chloroacetic acid in serum. Results The spiked recoveries of two concentrations of 200 μg / L and 1000 μg / L of chloracetic acid in serum were 85.6% and 91.5%, respectively. The intra-assay precision were 3.9% and 3.3%, respectively. The correlation coefficient was 0.9999; the lowest limit of quantification was 30μg / L, the lowest detected concentration was 10μg / L (with 1ml serum Meter), blood samples can be stored at 4 ℃ for 1 week, at -20 ℃ for 2 weeks. Conclusion The method of the technical indicators in line with the development of GBZ / T210.5-2008 specifications, can be used to detect occupational poisoning serum chloroacetate levels.