摘要
建立全自动固相萃取-气相色谱法同时测定地表水中20种多溴联苯的方法。水样经0.45μm滤膜过滤后用0.05 g/mL氢氧化钠溶液或盐酸溶液(体积比1∶1)调节pH至中性,加入10 mL甲醇作为有机改性剂混匀,通过全自动固相萃取仪以10 mL/min的流量上样,被测物质经PS/DVB固相萃取柱富集后,用正己烷-乙酸乙酯(体积比7∶3)混合溶剂洗脱。采用DB-5MS(15 m×0.25 mm,0.1μm)毛细管柱分离,电子捕获检测器检测,外标法定量。结果表明,20种多溴联苯的质量浓度在5.0~100μg/L范围内线性良好,相关系数均大于0.998,方法检出限为1.3~4.4 ng/L,定量限为5.2~17.6 ng/L,在20.0 ng/L和80.0 ng/L 2种添加水平下平均加标回收率为72.8%~90.9%,相对标准偏差为3.3%~8.5%。该方法自动化程度高、操作简便,具有良好的精密性和准确性,可以满足地表水中多溴联苯的快速测定要求。
A method for the simultaneous determination of 20 polybrominated biphenyls in surface water by automatic solid phase extraction-gas chromatography was established.The water sample was filtered through 0.45μm membrane,the sample pH was adjusted to neutral with 0.05 g/mL sodium hydroxide solution or hydrochloric acid solution(1/1,volume ratio),10 mL methanol was added as organic modifier,to be mixed with the sample,the sample was loaded with a flow rate of 10 mL/min through the automatic solid phase extraction instrument,the tested substance was eluted with a mixed solvent of n-hexane and ethyl acetate(7/3,volume ratio)after enrichment by PS/DVB solid phase extraction column.The extract was separated by DB-5MS(15 m×0.25 mm,0.1μm)capillary column,detected by electron capture detector,and quantified by external standard method.The results showed that the mass concentration of 20 kinds of polybrominated biphenyls had good linearity in the concentration range of 5.0 to 100μg/L,the correlation coefficients were all greater than 0.998,the method detection limits were 1.3 to 4.4 ng/L,and the quantification limits were 5.2 to 17.6 ng/L.The average spike recoveries at 20.0 ng/L and 80.0 ng/L spiked levels were 72.8%to 90.9%,and the relative standard deviations were 3.3%to 8.5%.The method has a high degree of automation,simple operation,good precision and accuracy,which can meet the requirements of rapid determination of PBBs in surface water.
作者
朱佩玉
高晨
姜金萍
顾俊鹏
ZHU Peiyu;GAO Chen;JIANG Jinping;GU Junpeng(Jiangsu Kangda Testing Technology Co.Ltd.,Suzhou 215000,China)
出处
《化学分析计量》
CAS
2023年第8期65-69,共5页
Chemical Analysis And Meterage
关键词
地表水
多溴联苯
全自动固相萃取
气相色谱法
surface water
polybrominated biphenyls
fully automatic solid phase extraction
gas chromatography
