Determination of 20 Organochlorine Pesticides and 7 Polychloro-Biphenyls in Sediments of Riverbank in Chemical Industry Area by Whole 2- Dimensional Gas Chromatography with Soxhlet Extraction
摘 要
取污染区沉积物,除去其中的异杂物后充分混匀。称取混匀样品10.00 g,加入适量经过在400℃烘烤4 h的无水硫酸钠并充分混合拌匀,研磨成细粒状。将此样品全部装入滤纸套筒中,并置于索氏提取器中,加入体积比为1:1的正己烷-丙酮混合溶液250 mL,在回流速率为10次·h-1条件下提取8~12 h (一般可采取多个样品同时提取过夜的操作方式)。收集所有提取液,混匀后将经活化处理的铜片置于此提取液中4~6 h除去硫化物。过滤除去沉淀,滤液浓缩后经以硅酸镁为载体的固相萃取柱净化。用体积比为9:1的正己烷-丙酮混合溶液15 mL洗脱固相萃取柱,收集洗脱液经浓缩至1.0 mL后,供色谱分离及测定。在此测定溶液中存在20种有机氯农药(OCPs)及7种多氯联苯(PCBs)共27种化合物。待测物在非极性一维TG-35MS色谱柱上按其沸点规律分离后,流出液经调制器聚焦后迅速升温(调制周期为4 s)并送入极性二维DB-1色谱柱按被测物的极性差异分离。两柱的组合达到上述27种化合物的良好分离。采用电子捕获检测器对27种化合物进行检测。上述27种化合物的质量浓度均在1.0~200.0 μg·L-1内与其对应的峰面积之间呈线性关系,其检出限(3.14s)为0.017~0.087 μg·kg-1。按标准加入法进行回收试验,测得回收率为72.0%~96.3%,测定值的相对标准偏差(n=6)为2.1%~11%。
Abstract
Sediment from riverbank of polluted area was collected and after picking out those impurities (i.e. branches, leaves, stones etc.) which were mixed up in, it was mixed thoroughly and ready to be used as analytical sample. 10.00 g of the sample were taken and mixed thoroughly with an appropriate amount of anhydrous Na2SO4, which has been baked at 400℃ for 4 h beforehand, and then ground to fine powdery state. The powder mixture was loaded completely into a sleeve made of filter paper, and the sleeve was replaced into the Soxhlet extractor, and extracted with 250 mL of a mixed solution of n-hexane and acetone with the volume ratio of 1:1 for 8-12 h at a refluxing rate of 10 times perhour (the authors propose to arrange the soxhlet extraction overnight in batches, by automation). The extracts were collected, combined and mixed thoroughly. A pre-activated copper sheet was placed into the combined extract for 4-6 h to eliminate sulfide by precipitation of sulfide on the copper sheet. The solution mixture was then filtered, and the filtrate was concentrated to a smaller volume and purified by passing through SPE column packed with Florisil. The analytes were adsorbed on SPE column and were eluted from the column by 15 mL of a mixed solution of n-hexane and acetone with the volume ratio of 9:1. The eluate was collected and evaporated to a definite volume 1.0 mL in which 27 compounds[i.e. 20 organochlorine pesticides (OCPs) and 7 polychloro-biphenyls (PCBs)] were contained and be further separated and determined with ECD. In the 2-dimensional gas chromatography separation, 2 chromatographic columns, i.e. the non-polar column (TG-35MS, the 1 st D) and the polar column (DB-1, the 2nd D) were used in combination. Among the 27 compounds, non-polar compounds were separated according to their differences in boiling points on the 1st D-column; the eluate from which was modulated by focusing to elevate its temperature rapidly (with gap of modulation of 4 s) and introduced into 2nd D-column through which the analysts with differences in polarities were separated. Good separation of the 27 compounds was attained by this arrangement. Linear relationships between values of mass concentration of the 27 compounds and their respective peak areas were found in the same range of 1.0-200.0 μg·L-1; with their detection limits (3.14 s) in the range of 0.017-0.087 μg·kg-1. Test for recovery was made by standard addition method, the results of recovery were found ranged from 72.0% to 96.3%, and values of RSDs (n=6) were found in the range from 2.1% to 11%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202001004
所属栏目 工作简报
基金项目 国家重点研发计划项目(2017YFF0206804)
收稿日期 2019/5/8
修改稿日期
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备注吕爱娟,工程师,硕士,研究方向为有机污染物分析检测,693541487@qq.com
引用该论文: Lü Aijuan,SHI Lei,SHEN Xiaoming,LIU Jiao,CAI Xiaohu. Determination of 20 Organochlorine Pesticides and 7 Polychloro-Biphenyls in Sediments of Riverbank in Chemical Industry Area by Whole 2- Dimensional Gas Chromatography with Soxhlet Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(1): 20~25
吕爱娟,时磊,沈小明,刘娇,蔡小虎. 索氏提取-全二维气相色谱法测定化工区江滩沉积物中20种有机氯农药和7种多氯联苯的含量[J]. 理化检验-化学分册, 2020, 56(1): 20~25
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参考文献
【1】高翔云,杨敏娜,刘秋香.气相色谱-质谱法测定沉积物中的有机氯和多氯联苯[J].环境监测管理与技术, 2015,27(3):48-51.
【2】张利,刘红玉,张慧,等.湖南东部地区稻田土壤中有机氯农药残留及分布[J].环境科学研究, 2008,21(1):118-123.
【3】时磊,陈海英,蔡小虎,等.超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯[J].理化检验-化学分册, 2016,52(9):1090-1094.
【4】徐宜宏,黄莹滢,裴程程,等.QuECHERS-气相色谱质谱法同时测定土壤中多种常见多氯联苯及有机氯农药[J].农药, 2018,57(5):351-354.
【5】蒙冰君,刘煜,王文涛,等.提取土壤中23种有机氯农药:微波法与索氏法对比[J].环境化学, 2007,26(6):854-855.
【6】张岩,张景发,陈艳梅,等.加速溶剂萃取-气相色谱法测定土壤中有机氯农药和多氯联苯[J].岩矿测试, 2010,29(5):491-496.
【7】郎印海,蒋新,赵振华,等.土壤中13种有机氯农药超声波提取方法研究[J].环境科学学报, 2004,24(2):291-296.
【8】包苏英,王瑞,徐琳燕,等.快速溶剂萃取-层析柱净化-气相色谱质谱法测定土壤中对苯二甲酸二(2-乙基己基)酯含量[J].浙江化工, 2018,49(8):45-50.
【9】张茜,刘潇威,罗铭,等.快速溶剂(ASE)提取、凝胶渗透色谱(GPC)联合固相萃取(SPE)净化,高效液相色谱法测定土壤中的多环芳烃[J].环境化学, 2011,30(4):771-777.
【10】林涛,邵金良,刘兴勇,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中41种农药残留[J].色谱, 2015,33(3):235-241.
【11】张兵,郑明辉,刘国瑞,等.全二维气相色谱-电子捕获检测器法分析土壤中毒杀芬同类物的残留[J].分析化学, 2012,40(8):1213-1218.
【12】时秋娜,刘占芳,朱军,等.全二维气相色谱-质谱法检测动植物油[J].中国油脂, 2017,42(6):138-142.
【13】童婷,张万峰,李东浩,等.气流吹扫-注射器微萃取-全二维气相色谱法用于原油组分的表征[J].色谱, 2014,32(10):1144-1151.
【2】张利,刘红玉,张慧,等.湖南东部地区稻田土壤中有机氯农药残留及分布[J].环境科学研究, 2008,21(1):118-123.
【3】时磊,陈海英,蔡小虎,等.超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯[J].理化检验-化学分册, 2016,52(9):1090-1094.
【4】徐宜宏,黄莹滢,裴程程,等.QuECHERS-气相色谱质谱法同时测定土壤中多种常见多氯联苯及有机氯农药[J].农药, 2018,57(5):351-354.
【5】蒙冰君,刘煜,王文涛,等.提取土壤中23种有机氯农药:微波法与索氏法对比[J].环境化学, 2007,26(6):854-855.
【6】张岩,张景发,陈艳梅,等.加速溶剂萃取-气相色谱法测定土壤中有机氯农药和多氯联苯[J].岩矿测试, 2010,29(5):491-496.
【7】郎印海,蒋新,赵振华,等.土壤中13种有机氯农药超声波提取方法研究[J].环境科学学报, 2004,24(2):291-296.
【8】包苏英,王瑞,徐琳燕,等.快速溶剂萃取-层析柱净化-气相色谱质谱法测定土壤中对苯二甲酸二(2-乙基己基)酯含量[J].浙江化工, 2018,49(8):45-50.
【9】张茜,刘潇威,罗铭,等.快速溶剂(ASE)提取、凝胶渗透色谱(GPC)联合固相萃取(SPE)净化,高效液相色谱法测定土壤中的多环芳烃[J].环境化学, 2011,30(4):771-777.
【10】林涛,邵金良,刘兴勇,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中41种农药残留[J].色谱, 2015,33(3):235-241.
【11】张兵,郑明辉,刘国瑞,等.全二维气相色谱-电子捕获检测器法分析土壤中毒杀芬同类物的残留[J].分析化学, 2012,40(8):1213-1218.
【12】时秋娜,刘占芳,朱军,等.全二维气相色谱-质谱法检测动植物油[J].中国油脂, 2017,42(6):138-142.
【13】童婷,张万峰,李东浩,等.气流吹扫-注射器微萃取-全二维气相色谱法用于原油组分的表征[J].色谱, 2014,32(10):1144-1151.
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