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  • Title: [Determination of trace perfluorinated compounds in environmental water samples by dispersive solid- phase extraction-high performance liquid chromatography-tandem mass spectrometry using carbon nanotube composite materials].
    Author: Song XL, Wang N, He FY, Cheng CL, Wang F, Wang JL, Zhang LH.
    Journal: Se Pu; 2023 May 08; 41(5):409-416. PubMed ID: 37087606.
    Abstract:
    In this work, carbon nanotubes (CNTs) on silica rod (SiO2) 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@SiO2, 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 5.0 μL. The chromatographic separation system was equipped with a Kinetex C18 column (100 mm×2.1 mm, 1.7 μm). The mass spectrometer was operated with negative electrospray ionization in multi-reaction monitoring mode. CNT@SiO2 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@SiO2 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. The method validation results indicated that the linear ranges were 0.4-1000 ng/L for PFNA, PFOS, and PFDA, 0.9-1000 ng/L for PFHpA, 0.7-1000 ng/L for PFHxS, and 0.6-1000 ng/L for PFOA. The correlation coefficients were 0.973-0.997. The limit of detection (LOD) and limit of quantification of the method were 0.10-0.26 ng/L and 0.33-0.87 ng/L, respectively. At 20 ng/L, the RSDs of the intra- and inter-day precisions were 2.73%-7.75% and 3.38%-8.21%, respectively. At 100 ng/L, the RSDs of the intra- and inter-day precisions were 2.95%-8.46% and 4.16%-9.14%, respectively. Finally, at 500 ng/L, the RSDs of the intra- and inter-day precisions were 2.51%-7.48% and 3.59%-9.63%, respectively. The developed method was applied to analyze six PFCs in tap water, barreled drinking water, and river water samples. PFOA and PFOS were determined in tap water at mass concentrations of 5.6 and 8.7 ng/L, respectively. No PFCs were found in barreled drinking water and river water. Satisfactory recoveries of 72.1%-109.6% at low, middle, and high spiking levels were also obtained. In conclusion, the d-SPE-LC-MS/MS method based on CNT@SiO2 composite sorbents is accurate and sensitive. The results of this study demonstrate that CNT@SiO2 is a good choice for the rapid and effective determination of PFCs from water samples. Further exploration of the use of CNT@SiO2 sorbents for the extraction and determination of trace organic pollutions in environmental samples is in progress. 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, 1.7 μm)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。
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