加压流体萃取-气相色谱法测定土壤中酞酸酯类化合物
|
摘要
建立了土壤中15种酞酸酯的加压流体萃取-弗罗里硅土柱净化-气相色谱测定方法。就萃取条件探讨了溶剂、温度、时间和循环次数对萃取效率的影响,就净化条件探讨了净化柱和洗脱溶剂对萃取效率的影响。根据研究结果,确定萃取条件以二氯甲烷为萃取溶剂,在萃取温度120℃、压强1 500 psi时,预热5 min,静态提取5 min,循环萃取2次,用体积为60%萃取池体积的萃取溶剂冲洗萃取池,之后用氮气吹扫萃取池90 s;净化条件为萃取溶液过弗罗里硅土固相萃取柱净化后,以正己烷∶丙酮(体积比为5∶1)洗脱。15种酞酸酯类化合物加标回收率为67.1%~124%,方法检出限为0.017~0.048 mg/kg。
A method was developed for the determination of 15 kinds of phthalate esters(APEs) in soil by pressurized fluid extraction,Florisil purification and gas chromatography in this study.The effects of extraction solvent,temperature,duration,repeating times,purification column and elution solvent on extraction efficiency were investigated in detail.The results showed that the optimized extraction procedures are circulating extraction of the soil twice with dichloromethane for 5 minutes at each time under the temperature of 120 ℃ degrees and the pressure of 1 500 psi after preheating for 5 minutes,purifying the solvent extract with Florisil column and eluting with Hexane∶Acetone(5∶1).The average recoveries for 15 kinds of APEs are 67.1%-124%,and the detection limits are 0.017-0.048 mg/kg.
A method was developed for the determination of 15 kinds of phthalate esters(APEs) in soil by pressurized fluid extraction,Florisil purification and gas chromatography in this study.The effects of extraction solvent,temperature,duration,repeating times,purification column and elution solvent on extraction efficiency were investigated in detail.The results showed that the optimized extraction procedures are circulating extraction of the soil twice with dichloromethane for 5 minutes at each time under the temperature of 120 ℃ degrees and the pressure of 1 500 psi after preheating for 5 minutes,purifying the solvent extract with Florisil column and eluting with Hexane∶Acetone(5∶1).The average recoveries for 15 kinds of APEs are 67.1%-124%,and the detection limits are 0.017-0.048 mg/kg.
引文
[1]PALACKVA J,JIRASEK J,PAUL A.The effect of sublethal anmonia concentration on selected physiological characteristics in carp(cyprinus carpio)[J].Zivocisna,Vyrora,1986,31(10):893-900.
[2]XIE Z,EBINGHAUS R,TEMME C,et al.Occurrence and air-sea exchange of phthalates in the Arctic[J].Environmental Science and Technology,2007,41:4 555-4 560.
[3]MELNICK R L.Is peroxisome proliferation an obligatory precursor step in the carcinogenicity of di(2-ethylhexyl)phthalate(DEHP)?[J].Environmental Health Perspectives,2001,109(5):437-44.
[4]ANDERSON D,YU T W,HINCAL F.Effect of some phthalate esters in human cells in the comet assay[J].Teratogenesis Carcinogenesis&Mutagenesis,1999,19(4):275-280.
[5]DEES J H,GAZOULI M,PAPADOPOULOS V.Effect of mono-ethylhexyl phthalate on MA-10 leydig tumor cells[J].Reproductive Toxicology,2001,15(2):171-187.
[6]DALGAARD M,NELLEMANN C,LAM H R,et al.The acute effects of mono(2-ethylhexyl)phthalate(MEHP)on testes of prepubertal wistar rats[J].Toxicol Lett,2001,122(l):69-79.
[7]冯碧,邵健忠.环境激素对动物生存的威胁[J].四川动物,2002,21(l):25-27.FENG Bi,SHAO Jianzhong.The threats of environmental hormones on animals[J].Sichuan Journal of Zoology,2002,21(l):25-27.
[8]邱东茹,吴振斌,贺锋.内分泌扰乱化学品对动物的影响和作用机制[J].环境科学研究,2000,13(6):52-55.QIU Dongru,WU Zhenbin,HE Feng.Effects of endocrine disrupting chemicals on animals and mechanisms of action[J].Research of Environmental Sciences,2000,13(6):52-55.
[9]陈永山,骆永明,章海波,等.土壤样品中酞酸酯含量分析的前处理研究[J].土壤学报,2011,48(2):311-319.CHEN Yongshan,LUO Yongming,ZHANG Haibo,et al.Pretreatment of soil samples for analysis of phthalate esters therein-effect of concentration and purification of the extract[J].Acta Pedologica Sinica,2011,48(2):311-319.
[10]周晓龙,刘河疆,钱宗耀,等.气相色谱法测定土壤中的6种酞酸酯[J].现代科学仪器,2011(6):136-137,140.ZHOU Xiaolong,LIU Hejiang,QIAN Zongyao,et al.Determination of the 6 phthalates in soil samples by GC[J].Modern Scientific Instruments,2011(6):136-137,140.
[11]李娟,赵永刚.微波萃取-高效液相色谱法测定土壤中的酞酸酯类化合物[J].科技资讯,2010(31):210,212.LI Juan,ZHAO Yonggang.Determination of phthalate esters in soil by microwave-assisted extraction and high performance liquid chromatography[J].Science Technology Information,2010(31):210,212.
[12]王盛才,胡华勇,罗岳平,等.GC-MS测定土壤中酞酸酯类化合物[J].中国环境监测,2007,23(4):23-25.WANG Shengcai,HU Huayong,LUO Yongping,et al.GC-MS determination of phthalates in soil samples[J].Environmental Monitoring in China,2007,23(4):23-25.
[13]罗财红,郭志顺,孙静.快速溶剂萃取-气相色谱-三重四极杆质谱法测定沉积物中的酞酸酯[J].色谱,2010,28(5):487-490.LUO Caihong,GUO Zhishun,SUN Jing.Determination of phthalate esters in sediment by accelerated solvent extraction and gas chromatographytriple quadrupole mass spectrometry[J].Chinese Journal of Chromatography,2010,28(5):487-490.
[14]环境保护部科技标准司.环境监测分析方法标准制修订技术导则:HJ 168-2010[S].北京:中国环境科学出版社,2010.
[2]XIE Z,EBINGHAUS R,TEMME C,et al.Occurrence and air-sea exchange of phthalates in the Arctic[J].Environmental Science and Technology,2007,41:4 555-4 560.
[3]MELNICK R L.Is peroxisome proliferation an obligatory precursor step in the carcinogenicity of di(2-ethylhexyl)phthalate(DEHP)?[J].Environmental Health Perspectives,2001,109(5):437-44.
[4]ANDERSON D,YU T W,HINCAL F.Effect of some phthalate esters in human cells in the comet assay[J].Teratogenesis Carcinogenesis&Mutagenesis,1999,19(4):275-280.
[5]DEES J H,GAZOULI M,PAPADOPOULOS V.Effect of mono-ethylhexyl phthalate on MA-10 leydig tumor cells[J].Reproductive Toxicology,2001,15(2):171-187.
[6]DALGAARD M,NELLEMANN C,LAM H R,et al.The acute effects of mono(2-ethylhexyl)phthalate(MEHP)on testes of prepubertal wistar rats[J].Toxicol Lett,2001,122(l):69-79.
[7]冯碧,邵健忠.环境激素对动物生存的威胁[J].四川动物,2002,21(l):25-27.FENG Bi,SHAO Jianzhong.The threats of environmental hormones on animals[J].Sichuan Journal of Zoology,2002,21(l):25-27.
[8]邱东茹,吴振斌,贺锋.内分泌扰乱化学品对动物的影响和作用机制[J].环境科学研究,2000,13(6):52-55.QIU Dongru,WU Zhenbin,HE Feng.Effects of endocrine disrupting chemicals on animals and mechanisms of action[J].Research of Environmental Sciences,2000,13(6):52-55.
[9]陈永山,骆永明,章海波,等.土壤样品中酞酸酯含量分析的前处理研究[J].土壤学报,2011,48(2):311-319.CHEN Yongshan,LUO Yongming,ZHANG Haibo,et al.Pretreatment of soil samples for analysis of phthalate esters therein-effect of concentration and purification of the extract[J].Acta Pedologica Sinica,2011,48(2):311-319.
[10]周晓龙,刘河疆,钱宗耀,等.气相色谱法测定土壤中的6种酞酸酯[J].现代科学仪器,2011(6):136-137,140.ZHOU Xiaolong,LIU Hejiang,QIAN Zongyao,et al.Determination of the 6 phthalates in soil samples by GC[J].Modern Scientific Instruments,2011(6):136-137,140.
[11]李娟,赵永刚.微波萃取-高效液相色谱法测定土壤中的酞酸酯类化合物[J].科技资讯,2010(31):210,212.LI Juan,ZHAO Yonggang.Determination of phthalate esters in soil by microwave-assisted extraction and high performance liquid chromatography[J].Science Technology Information,2010(31):210,212.
[12]王盛才,胡华勇,罗岳平,等.GC-MS测定土壤中酞酸酯类化合物[J].中国环境监测,2007,23(4):23-25.WANG Shengcai,HU Huayong,LUO Yongping,et al.GC-MS determination of phthalates in soil samples[J].Environmental Monitoring in China,2007,23(4):23-25.
[13]罗财红,郭志顺,孙静.快速溶剂萃取-气相色谱-三重四极杆质谱法测定沉积物中的酞酸酯[J].色谱,2010,28(5):487-490.LUO Caihong,GUO Zhishun,SUN Jing.Determination of phthalate esters in sediment by accelerated solvent extraction and gas chromatographytriple quadrupole mass spectrometry[J].Chinese Journal of Chromatography,2010,28(5):487-490.
[14]环境保护部科技标准司.环境监测分析方法标准制修订技术导则:HJ 168-2010[S].北京:中国环境科学出版社,2010.