磁性氯甲基聚苯乙烯微球固相萃取-气相色谱-串联质谱法测定环境水样中7种硝基苯类化合物
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摘要
采用磁性氯甲基聚苯乙烯微球(CMPNs)固相萃取-气相色谱-串联质谱法测定环境水样中7种硝基苯类化合物(NBs)的含量。优化的试验条件如下:(1)萃取剂为CMPNs材料;(2)CMPNs的用量为15.0mg;(3)萃取时间为4min;(4)氯化钠的加入量为340g·L~(-1);(5)洗脱剂丙酮的用量为3mL;(6)洗脱时间为1min。气相色谱分离用HP-INNOWAX色谱柱,质谱分析采用全扫描和选择离子监测模式。7种NBs的质量浓度均在0.2~4.0μg·L~(-1)内与其峰面积呈线性关系,方法的检出限(3S/N)在0.006~0.022μg·L~(-1)之间。7种NBs测定值的相对标准偏差(n=6)在0.30%~5.3%之间。方法用于环境水样的分析,回收率在72.4%~113%之间。
GC-MS/MS was applied to the determination of 7nitrobenzenes in environmental water samples with solidphase extraction based on chloromethylated magnetic polystyrene nanospheres(CMPNs).The optimized conditions found were as follows:(1) extracting agent:CMPNs material;(2) amount of CMPNs:15.0 mg;(3)extraction time:4min;(4) amount of NaCl:340g·L~(-1);(5) amount of acetone(eluant):3mL;(6) elution time:1min.The HP-INNOWAX chromatographic column was used for GC separation,and the full-scanning mode and the selected ion monitoring mode were adopted in MS.Linear relationships between values of peak area and mass concentration of the 7nitrobenzenes were kept in the same range of 0.2-4.0μg·L~(-1),with detection limits(3S/N)in the range of 0.006-0.022μg·L~(-1).Precision of the method was tested,and values of RSD(n=6)for7NBs found were in the range of 0.30%-5.3%.The proposed method was applied to the analysis of environmental water samples,giving values of recovery in the range of 72.4%-113%.
GC-MS/MS was applied to the determination of 7nitrobenzenes in environmental water samples with solidphase extraction based on chloromethylated magnetic polystyrene nanospheres(CMPNs).The optimized conditions found were as follows:(1) extracting agent:CMPNs material;(2) amount of CMPNs:15.0 mg;(3)extraction time:4min;(4) amount of NaCl:340g·L~(-1);(5) amount of acetone(eluant):3mL;(6) elution time:1min.The HP-INNOWAX chromatographic column was used for GC separation,and the full-scanning mode and the selected ion monitoring mode were adopted in MS.Linear relationships between values of peak area and mass concentration of the 7nitrobenzenes were kept in the same range of 0.2-4.0μg·L~(-1),with detection limits(3S/N)in the range of 0.006-0.022μg·L~(-1).Precision of the method was tested,and values of RSD(n=6)for7NBs found were in the range of 0.30%-5.3%.The proposed method was applied to the analysis of environmental water samples,giving values of recovery in the range of 72.4%-113%.
引文
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[2]GB 22573-2008灌溉水中氯苯、1,2-二氯苯、1,4-二氯苯、硝基苯限量[S].
[3]WU L J,SONG C M,ZHAO Y,et al.Determination of organochlorine pesticides in tea beverage by directly suspended droplet microextraction combined with GCECD[J].Food Anal Method,2015,8(1):147-153.
[4]CORTADA C,VIDAL L,CANALS A.Determination of nitroaromatic explosives in water samples by direct ultrasound-assisted dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry[J].Talanta,2011,85(5):2546-2552.
[5]张营,郜炜,景逵,等.液液萃取-气相色谱法测定水中的硝基苯类化合物[J].辽宁大学学报(自然科学版),2010,37(3):282-284.
[6]刘宁.固相萃取-气相色谱法测定水中硝基苯类化合物的含量[J].山东化工,2012,41(5):48-51.
[7]PENG X T,XING Z,FENG Y Q.Preparation of phenothiazine bonded silica gel as sorbents of solid phase extraction and their application for determination of nitrobenzene compounds in environmental water by gas chromatography-mass spectrometry[J].J Chromatogr A,2011,1218:9314-9320.
[8]任朝兴,向统领,杨家欢.固相萃取-气相色谱/质谱法同时测定海水中9种硝基苯类化合物[J].海洋环境科学,2012,31(5):743-745.
[9]XIE F W,SHANG J J,GUO J Z,et al.Determination of seven nitrobenzene compounds in mainstream cigarette smoke with heart-cutting two-dimensional gas chromatography[J].J Chromatogr A,2012,50:387-392.
[10]任衍燕.固相萃取-气相色谱/质谱法测定水中硝基苯类化合物[J].城镇供水,2012(5):51-52.
[11]刁春鹏,赵汝松,柳仁民,等.分散液相微萃取-气相色谱/质谱快速分析水中的硝基苯类化合物[J].分析试验室,2009,28(6):9-12.
[12]翦英红,范宁伟,张德.分散液液微萃取高效液相色谱法测定环境水样中硝基苯[J].天津化工,2011,25(1):51-53.
[13]沈彬,罗三姗,张占恩.液相微萃取-气相色谱/质谱测定水中硝基苯类化合物[J].分析科学学报,2007,23(6):705-708.
[14]CHA D M,MA B.Determination of nitrobenzene in water using ionic liquid-based liquid-phase microextraction coupled with HPLC[J].American Laboratory,2009,41:12-15.
[15]YAO C,TWU P,ANDERSON J L.Headspace single drop microextraction using micellar ionic liquid extraction solvents[J].Chromatographia,2010,72:393-402.
[16]母应锋,杨丽莉,胡恩宇,等.一滴溶剂微萃取-毛细管气相色谱法分析水中的七种硝基苯类化合物[J].色谱,2007,25(6):876-880.
[17]CAO X J,SHEN L X,YE X M,et al.Ultrasoundassisted magnetic solid-phase extraction based ionic liquid-coated Fe3O4@graphene for the determination of nitrobenzene compounds in environmental water samples[J].Analyst,2014,139(8):1938-1944.
[18]ZHENG Z,WANG J L,ZHANG M,et al.Magnetic polystyrene nanosphere immobilized TEMPO:a readily prepared,highly reactive and recyclable polymer catalyst in the selective oxidation of alcohols[J].Chem Cat Chem,2013,5(1):307-312.
[19]CAO X J,KONG Q L,CAI R N,et al.Solid-phase extraction based on chloromethylated polystyrene magnetic nanospheres followed by gas chromatography with mass spectrometry to determine phthalate esters in beverages[J].J Sep Sci,2014,37(24):3677-3683.