首页|固相萃取填料对水中脂肪族二元酸酯类增塑剂萃取效率的影响

固相萃取填料对水中脂肪族二元酸酯类增塑剂萃取效率的影响

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以水中 11 种脂肪族二元酸酯类(ADEs)增塑剂的固相萃取-气相色谱-质谱法(SPE-GC-MS)为例,探讨了用 C18柱和 HLB柱萃取水样时不同品牌、不同批号的 SPE填料和 C18 柱封端与否及相对应的洗脱溶剂不同配比对萃取效率的影响.实验结果表明:正己烷不可作为 C18 柱和 HLB柱的淋洗溶剂;11 种 ADEs用不同配比的二氯甲烷/正己烷溶剂体系洗脱,对 C18 柱和 HLB柱,不同 SPE填料最佳二氯甲烷体积分数分别为 0~60%和 15%~20%;未经封端处理的 C18 柱不适合作为 ADEs的 SPE柱;最佳溶剂洗脱体积为 5 mL,样品穿透体积至少为 200 mL;在优化条件下,11 种 ADEs 方法检出限为 0.2~0.5 μg/L,实际样品加标回收率为 85.2%~113%,平行样相对标准偏差为 5.5%~18%,各特性指标显示该方法正确度、精密度和灵敏度良好.
Influence of Solid Phase Extraction Sorbents on Extraction Efficiency of Aliphatic Dicarboxylate Esters Plasticizer in Water
Taking the inspection method of 11 aliphatic dicarboxylate esters plasticizers in water by the solid phase extraction-gas chromatography-mass spectrometry(SPE-GC-MS)as an example,the effects of different brands,batches of SPE sorbents,C18 column and the corresponding ratio of eluting solvents on the extraction efficiency of water samples with C18 column and HLB column were discussed.The results showed that n-hexane could not be used as the wash solvent of C18 columns and HLB columns.The optimum dichloromethane content ratios of dichloromethane/n-hexane eluting solvent system for 11 ADEs with different SPE sorbents of C18 column and HLB were 0-60%and 15%-20%respectively.C18 column without capping treatment was not suitable for SPE of ADEs.The optimal solvent elution volume was 5 mL,and the sample breakthrough volume was at least 200 mL.Under the optimized conditions,the method detection limits(MDLs)of the 11 ADEs methods were 0.2-0.5 μg/L,the recoveries of spiked actual water sample were 85.2%-113%,and the relative standard deviations(RSDs)of the parallel samples were 5.5%-18%,which indicating that the proposed method was efficient,accurate and sensitive.

solid phase extraction(SPE)sorbentaliphatic dicarboxylate esters(ADEs)extraction efficiencygas chromatographymass spectrometrywater samples

李利荣、左明、王迎、王洪乾、刘殿甲、张肇元、王效国

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天津市生态环境监测中心,天津 300191

固相萃取填料 脂肪族二元酸酯 萃取效率 气相色谱 质谱法 水样

国家环境保护标准制修订项目

2021-12

2024

中国环境监测
中国环境监测总站

中国环境监测

CSTPCD北大核心
影响因子:1.761
ISSN:1002-6002
年,卷(期):2024.40(2)
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