摘要
以碳纳米管-二氧化硅棒复合材料为吸附剂,基于分散固相萃取法和液相色谱-串联质谱法建立了一种高灵敏、快速分析环境水样中痕量全氟化合物(PFCs)的方法。该研究选择全氟己烷磺酸、全氟庚酸、全氟辛酸、全氟辛烷磺酸、全氟壬酸和全氟癸酸6种全氟化合物为目标分析物。采用单因素优化法对影响萃取效果的重要因素进行了优化。获得的最佳条件为:吸附时间为30 min、吸附剂用量为10 mg、样品溶液pH为6、萃取过程添加NaCl浓度为1.7 mol/L、解吸溶剂为丙酮、解吸时间为4 min、解吸液的体积为4 mL。采用高效液相色谱-三重四极杆质谱联用技术对水样品中全氟化合物进行定量分析。以5 mmol/L乙酸铵和甲醇为流动相进行梯度洗脱,经Kinetex C18色谱柱(100 mm×2.1 mm, 1.7μm)分离,采用电喷雾离子源、负离子扫描模式和质谱多反应监测,实现了环境水样中6种全氟化合物的快速定性和定量分析。在优化条件下,6种全氟化合物在各自的线性范围内线性关系良好,检出限(S/N=3)为0.10~0.26 ng/L。添加500 ng/L 6种PFCs进行重复性实验,日内相对标准偏差(RSD)为2.51%~7.48%,日间RSD为3.59%~9.63%。将方法应用于自来水、桶装饮用水和河水3种实际环境水样中全氟化合物的分析,在低、中、高3个水平下,6种全氟化合物的加标回收率为72.1%~109.6%,结果满意。本方法成功地应用于实际环境水样中全氟化合物的检测,为快速、有效地检测环境水样中痕量全氟化合物提供了良好的选择。
In this work,carbon nanotubes(CNTs)on silica rod(SiO 2)composite materials were prepared to extract six perfluorinated compounds(PFCs)in real environmental water samples by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The as-synthesized sorbents,hereafter referred to as CNT@SiO 2,were employed for dispersive solid-phase extraction(d-SPE).Perfluoroheptanoic acid(PFHpA),perfluorohexane sulfonate(PFHxS),perfluorooctanoic acid(PFOA),perfluorononanoic acid(PFNA),perfluorooctane sulfonate(PFOS),and perfluorodecanoic acid(PFDA)were selected as target analytes.The main extraction parameters were systematically optimized using the single-factor optimization method.The optimum adsorption parameters were as follows:adsorption time of 30 min,sorbent amount of 10 mg,pH 6 and NaCl concentration of 1.7 mol/L for sample solution,and 4 mL acetone as desorption solvent,desorption for 4 min.LC-triple quadrupole MS was conducted to quantify the selected PFCs in water samples.The mobile phase was 5 mmol/L ammonium acetate and methanol,the flow rate was set to 0.4 mL/min,the column temperature was set to 40℃,and the injection volume was 5.0μL.The chromatographic separation system was equipped with a Kinetex C18 column(100 mm×2.1 mm,1.7μm).The mass spectrometer was operated with negative electrospray ionization in multi-reaction monitoring mode.CNT@SiO 2 was prepared in five batches and used as the d-SPE sorbent,and the relative standard deviations(RSDs)of the PFC recoveries among these five batches ranged from 4.9%to 9.3%.The reusability of the CNT@SiO 2 sorbent was assessed.After eight d-SPE cycles using the same sorbent,the RSDs of the PFC recoveries were 3.7%-8.2%.These results indicated that the sorbent had good stability and reusability for d-SPE.Excellent results were achieved under optimal extraction conditions.CNT@SiO 2 showed wide linear ranges,low limits of detection(LODs),and good repeatability for detecting and extracting the six PFCs.The method validation results indicated that the line
作者
宋新力
王宁
何飞燕
程灿玲
王飞
王京龙
张立华
SONG Xinli;WANG Ning;HE Feiyan;CHENG Canling;WANG Fei;WANG Jinglong;ZHANG Lihua(College of Food Science and Pharmaceutical Engineering,Zaozhuang University,Zaozhuang 277160,China)
出处
《色谱》
CAS
CSCD
北大核心
2023年第5期409-416,共8页
Chinese Journal of Chromatography
基金
枣庄市科技计划项目(2021GX09)。
关键词
碳纳米管复合材料
分散固相萃取
液相色谱-串联质谱
全氟化合物
环境水样
carbon nanotube composite materials
dispersive solid-phase extraction(d-SPE)
liquid chromatography-tandem mass spectrometry(LC-MS/MS)
perfluorinated compounds(PFCs)
environmental water sample
