摘要
提出了固相萃取-衍生化-气相色谱-质谱法同时测定环境水中双酚A(BPA)和9种C4~C9烷基酚类化合物(APs,包括4-叔丁基苯酚、4-丁基苯酚、4-戊基苯酚、4-己基苯酚、4-叔辛基苯酚、4-庚基苯酚、壬基酚、4-辛基苯酚和4-壬基苯酚)含量的方法。取500 mL水样,用50%(体积分数)盐酸溶液调节pH小于2,以50 mL·min^(-1)速率通过以苯乙烯/二乙烯苯聚合物为吸附剂的SDB-XC固相萃取膜,用5 mL丙酮和10 mL二氯甲烷洗脱。收集洗脱液,加入1 mL正己烷,经10 g无水硫酸钠脱水,用旋转蒸发仪浓缩至约0.5 mL后转移至1 mL容量瓶中。用少量二氯甲烷洗涤浓缩瓶,将洗涤液合并至容量瓶中,再依次加入100μL内标混合溶液和100μL衍生试剂,用二氯甲烷定容至1 mL,室温衍生1 h。上述溶液中各目标物在气相色谱仪中以程序升温和程序升压方式分离,在质谱仪中以选择离子监测模式测定,内标法定量。结果显示:BPA和9种APs标准曲线的线性范围为5.000~500.0μg·L^(-1),检出限为0.002~0.006μg·L^(-1);各目标物在空白加标水样中测定值的相对标准偏差(n=6)为1.2%~15%;方法用于实际地表水、生活污水和工业废水分析,均检出壬基酚和BPA,地表水和生活污水中还检出4-叔辛基苯酚,检出量为0.005~0.657μg·L^(-1),其余APs未检出,实际样品中BPA和9种APs的加标回收率为73.4%~125%。
A method for the simultaneous determination of bisphenol A(BPA)and 9 C4-C9 alkylphenols(APs,including 4-tert-butylphenol,4-n-butylphenol,4-n-pentylphenol,4-n-hexylphenol,4-tert-octylphenol,4-n-heptylphenol,nonylphenol,4-n-octylphenol and 4-n-nonylphenol)in environmental water by gas chromatography-mass spectrometry with solid phase extraction and derivatization was proposed.Water sample(500 mL)was adjusted pH to less than 2 with 50%(φ)hydrochloric acid solution,passed through solid phase extraction membrane with styrene/divinylbenzene polymer as adsorbent at the rate of 50 mL·min^(-1),and eluted with 5 mL of acetone and 10 mL of dichloromethane.The eluate was collected,and 1 mL of n-hexane was added.The mixture was dehydrated with 10 g of anhydrous sodium sulfate,and concentrated to about 0.5 mL by rotary evaporator.The concentrated solution was transferred to 1 mL-volumetric flask.The concentration bottle was washed with a small amount of dichloromethane,and the washing liquid was combined into the volumetric flask.Then 100μL of internal standard mixed solution and 100μL of derivative reagent were added successively,and the volume was made up to 1 mL with dichloromethane.The targets were derived at room temperature for 1 h.The targets in the above solution were separated by gas chromatograph with programmed temperature and programmed pressure,determined by mass spectrometer with selective ion monitoring mode,and quantified by internal standard method.As shown by the results,the linear ranges of standard curves of BPA and 9 APs were 5.000-500.0μg·L^(-1),with detection limits in the range of 0.002-0.006μg·L^(-1).RSDs(n=6)of the determined values of the targets in the blank water samples were in the range of 1.2%-15%.This method was applied to the analysis of surface water,sanitary sewage and industrial wastewater,in which nonylphenol and BPA were detected,and 4-tert-octylphenol was detected in the surface water and sanitary sewage,with detection amounts in the range of 0.005-0.657μg·L^(-1).The other APs
作者
周同娜
尹海亮
ZHOU Tongna;YIN Hailiang(Dongying Ecological Environment Monitoring Center of Shandong Province,Dongying 257091,China;Dongying Academy of Science&Technology,China University of Petroleum,Dongying 25706l,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2022年第10期1182-1188,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家环境保护标准制修订项目(2014-31)
东营市科技发展指导计划项目(2021ZD48)。
关键词
固相萃取
衍生
气相色谱-质谱法
水
双酚A
烷基酚类化合物
solid phase extraction
derivatization
gas chromatography-mass spectrometry
water
bisphenol A
alkylphenol
