| 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 |
| Influence of Solid Phase Extraction Sorbents on Extraction Efficiency of Aliphatic Dicarboxylate Esters Plasticizer in Water |
| 投稿时间：2022-10-25 修订日期：2023-02-15 |
| DOI：10.19316/j.issn.1002-6002.2024.02.20 |
| 中文关键词: 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 |
| 英文关键词:solid phase extraction (SPE) sorbent aliphatic dicarboxylate esters (ADEs) extraction efficiency gas chromatography mass spectrometry water samples |
| 基金项目:国家环境保护标准制修订项目(2021-12) |
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| 通讯作者:王迎* 天津市生态环境监测中心, 天津 300191 |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| Taking the inspection method of 11 aliphatic dicarboxylate esters plasticizers in water by the solid phase extractiongas 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 C 18 columns and HLB columns. The optimum dichloromethane content ratios of dichloromethane/n-hexane eluting solvent system for 11 ADEs with different SPE sorbents of C 18 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. |
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