摘要
建立了气相色谱-质谱联用仪法测定土壤/沉积物样品中苯胺、3,3’-二氯联苯胺的测定方法,采用半自动索氏提取前处理,使用萃取剂二氯甲烷-丙酮(体积比1∶1)对样品进行提取,对提取液净化、浓缩、定容,经气相色谱分离、质谱检测,根据保留时间、碎片离子质荷比及其丰度定性,内标法定量。结果表明:该方法在1.0~20.0 mg/L范围内线性良好,线性相关系数r>0.996,检出限均为0.02 mg/kg,测定下限均为:0.08 mg/kg;测定低、中、高三种浓度,土壤样品回收率范围分别为:58.3%~110%,63.9%~96.7%,63.7%~114%,相对标准偏差范围分别为:3.7%~8.0%,11.1%~14.5%,8.1%~2.6%,沉积物样品回收率范围分别为:64.2%~92.8%,78.2%~115%,59.0%~109%,相对标准偏差范围分别为:6.2%~6.4%,6.9%~7.1%,3.4%~14.2%。该方法成本低、准确可靠、操作简单、检出限低、精密度良好、回收率高,可以应用于实际土壤/沉积物样品中苯胺、3,3’-二氯联苯胺的检测。
This study established a method for the determination of aniline and 3,3'-dichlorobenzidine in soil/sediment samples using gas chromatography-mass spectrometry(GC-MS).The samples were pretreated by semi-automatic Soxhlet extraction with a mixed solvent of dichloromethane and acetone(1∶1)for extraction.The extract was then purified,concentrated,and reconstituted before GC separation and MS detection.Qualitative analysis was based on retention time,fragment ion mass-to-charge ratio(m/z),and abundance ratio,while quantitative analysis was performed using the internal standard method.The results showed good linearity within the range of 1.0~20.0 mg/L,with correlation coefficients(r)>0.996.The method detection limits(MDLs)were both 0.02 mg/kg,and the lower limits of quantification(LLOQs)were 0.08 mg/kg.For soil samples,the recoveries at low,medium,and high spiked concentrations were 58.3%~110%,63.9%~96.7%,and 63.7%~114%,respectively,with relative standard deviations(RSD)of 3.7%~8.0%,11.1%~14.5%,and 8.1%~2.6%.For sediment samples,the recoveries were 64.2%~92.8%,78.2%~115%,and 59.0%~109%,with RSD of 6.2%~6.4%,6.9%~7.1%,and 3.4%~14.2%.This method is cost-effective,accurate,reliable,easy to operate,and exhibits low detection limits,good precision,and high recovery rates,making it suitable for the determination of aniline and 3,3'-dichlorobenzidine in real soil and sediment samples.
作者
路艳芳
LU Yanfang(Shanghai Geotechnical Investigation&Surveying Co.,Ltd.,Shanghai 200346,China)
出处
《山东化工》
2025年第14期148-152,共5页
Shandong Chemical Industry
