液液小体积萃取气相色谱法分析水中丙烯酰胺.docVIP

双柱双检测器同时测定污染土壤中有机氯和多氯联苯 陈蓓蓓* （上海市环境监测中心，上海，200030） 摘 要：建立了超声波萃取-气相色谱法双柱双检测器同时测定污染土壤中23种有机氯和7组Aroclor的方法。用二氯甲烷超声萃取同时提取有机氯和多氯联苯，根据目标化合物选择相应的净化方法（SPE小柱、浓硫酸净化GPC）和定性定量方法采用双柱双μ-ECD测定，提高定性的准确性。当土壤取样量为20g，OCPs方法检出限为0.001mg/kg，平均回收率为82.1%~103%，相对标准偏差为1.8%~13%；Aroclor方法检出限为0.005mg/kg，平均回收率为83.5%~94.7%，相对标准偏差为1.8%~5.8%。 关键词：有机氯农药；多氯联苯；双柱双检测器；污染土壤；净化 Determination of Organochlorine Pesticides in Contaminated Soil by Gas Chromatography with Dual-Column and Dual-ECD CHEN Bei-bei （Shanghai Environmental Monitoring Centre, Shanghai 200030, China)Abstract：ethods for simultaneous determination of 23 organochlorine pesticides and 7 Aroclors in contaminated soil by ultrasonic extraction-gas chromatography combined with dual-column and dual-ECD was proposed. OCPs and PCBs were extracted simultaneously by ultrasonic extractor with CH2Cl2. According to the analytes, different cleanup methods including SPE cleanup, Sulfuric acid cleanup and GPC were chosen to remove the interferences. Dual-column and dual-ECD system were used to improve the accuracy of qualitative analysis. LMD of OCPs and Aroclor were 0.001mg/kg and 0.005mg/kg. Average recovery were between the range of 82.1%~103% and 83.5%~94.7%. Relative standard deviation were 1.8%~13% and 1.8%~5.8%. Keywords：Organochlorine Pesticides; Dual-Column and Dual-ECD; Contaminated Soil; Cleanup 有机氯农药( Organochlorine Pesticides，OCPs)是持久性有机污染物，具有“三致”。 土壤中OCPs检测方法主要有气相色谱法[-6] 、气质联用法[-12]和气相色谱串联质谱法[13,14]。相比于单色谱柱假阳性判断定性。本文OCPs和7组Aroclor为研究对象，参考美国EPA 方法8081B[15]和8082A[16]，建立了同时检测土壤中OCPs和Aroclor的前处理方法和分析方法。根据目标化合物，进一步优化了净化方法和定性定量方法，能快速准确地同时测定土壤中的OCPs和Aroclor，并已较好地运用于实际污染土壤的测定。 试验 1.1 仪器与试剂 7890气相色谱仪μ-ECD；Model500型探针式超声波提取仪TurboVapⅡ型氮吹浓缩仪色谱柱DB-170130m×0.53mm×1.0μm)，DB-5(30m×0.53mm×0.88μm)。 20种OCPs标准α-六六六β-六六六γ-六六六δ-六六六七氯艾氏剂γ-氯丹α-氯丹硫丹Ⅰ硫丹Ⅱ狄氏剂异狄氏剂p,p-滴滴依p,p-滴滴滴p,p-滴滴涕环氧七氯异狄氏剂醛异狄氏剂酮硫丹硫酸盐甲氧氯OCPs单标溶液（六氯苯、o,p-滴滴涕示踪物标准四氯间二甲苯十氯联苯铜粉农残级1.2 仪器工作条件 程序升温：10℃(1min)→15℃/min→160℃(2min)→3℃/min→180℃(12min)→4℃/min→230℃→5℃/min→270℃(8min)；进样口250℃；分流；检测器320℃；N2流量7