印染废水中全氟辛烷磺酸和全氟辛酸含量的液相色谱串联质谱测定  

Determination of perfluorooctane sulfonic acid and perfluorooctanoic acid contents in dyeing wastewater by LC-MS/MS

作　　者：李志刚[1] 杨宏林[1] LI Zhigang;YANG Honglin(Zhejiang Industry Polytechnic College,Shaoxing 312000,China)

机构地区：[1]浙江工业职业技术学院,浙江绍兴312000

出　　处：《印染》2024年第12期66-69,共4页China Dyeing and Finishing

基　　金：2022年绍兴市级科技计划项目(2022A11007);2022年浙江省高校国内访问工程师“校企合作项目”(FG2022212)。

摘　　要：建立了液相色谱串联质谱法测定纺织废水中全氟辛烷磺酸和全氟辛酸含量的方法。样品采用全自动固相萃取技术进行提取、净化和浓缩,过WAX固相萃取柱后,用2%氨水/甲醇洗脱,色谱柱为Waters ACQUITY UPLC BEH C18柱(100 mm×2.1 mm,1.7μm),1 mmol/L乙酸铵溶液和甲醇为流动相,以电喷雾负离子MRM模式进行检测,内标法定量。全氟辛烷磺酸和全氟辛酸在0.5~50.0μg/L质量浓度范围内均具有良好的线性关系,相关系数(R)均大于0.999,方法的检出限均为0.17 ng/L,定量限均为0.5 ng/L,平均加标回收率分别为94.1%和92.8%,精密度分别为2.6%~4.2%和3.1%~6.6%。该方法具有灵敏度高、准确度好的特点,可以为印染废水的日常监测管控提供技术支撑。A method for determination of perfluorooctane sulfonate and perfluorooctanoic acid in textile wastewater by liquid chromatography-tandem mass spectrometry is established.The sample is extracted,purified,and concentrated using automated solid-phase extraction technology.After passing through the WAX solidphase extraction column,the sample is washed with 2%ammonia/methanol solution.The samples are separated by Waters ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)with a linear gradient elution program of methanol and water(1 mmol/L ammonium acetate)as the mobile phase.The analytes are measured by using electrospray ion(ESI)in the negative multiple reaction monitoring(MRM)mode.Quantification is carried out by internal standard method.A good linearity is obtained in the concentration range of 0.5-50.0μg/L for target compounds with the correlation coefficients over 0.999.The limits of detection(LODs)and the limits of quantitation(LOQs)are 0.17 ng/L and 0.5 ng/L.The average spiked recoveries are 94.1%and 92.8%,the precisions are 2.6%-4.2%and 3.1%-6.6%,respectively.The established method has the characteristics of high sensitivity and good accuracy,which can provide technical support for the daily monitoring and control of printing and dyeing wastewater.

关 键 词：测试 液相色谱串联质谱 全自动固相萃取 全氟辛烷磺酸 全氟辛酸 印染废水 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]