首页|顶空固相微萃取-气质联用法测定水中4种痕量环状缩醛类异嗅物质

顶空固相微萃取-气质联用法测定水中4种痕量环状缩醛类异嗅物质

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文章采用顶空固相微萃取-气质联用技术,建立了水中2,2-二甲基-1,3-二氧环戊烷(22-DMD)、2-乙基-4-甲基-1,3-二氧戊环(2-EMD)、2-乙基-2-甲基-1,3-二氧戊环(2E2MD)、2-乙基-5,5-二甲基-1,3-二氧杂环乙烷(2-EDD)4种痕量环状缩醛类异嗅物质的检测方法。方法中固相微萃取前处理过程使用85 μm Carboxen/PDMS萃取纤维,萃取温度为60℃,萃取时间为25 min,盐析剂氯化钠添加的质量分数为20%,色谱分离过程使用Agilent DB-5MS气相色谱柱(60 mx0。25 mm× 1。00 μm),内标物使用2-异丁基-3-甲氧基吡嗪。22-DMD、顺式2-EMD、反式2-EMD、2E2MD、2-EDD的方法检出限分别为1。6、0。6、0。5、1。0、0。3 ng/L,纯水、水源水、水厂出厂水和管网水平行加标样品中4种环状缩醛类物质的相对标准偏差为1。6%~8。6%,加标回收率为94%~117%,方法特性指标均满足水中痕量环状缩醛类异嗅物质的测定需要。
Trace Level Quantification of Four Cyclic Acetals Odorous Compounds in Water by Use of Headspace SPME Followed by GC-MS
A detection method had been established for trace level analysis of 2,2-dimethyl-1,3-dioxolane(22-DMD),2-ethyl-4-methyl-1,3-dioxolane(2-EMD),2-ethyl-2-methyl-1,3-dioxolane(2E2MD),2-ethyl-5,5-dimethyl-1,3-dioxane(2-EDD),totally four cyclic acetals odorous compounds in water by use of headspace SPME followed by GC-MS.In SPME pretreatment period,85 μm Carboxen/PDMS fiber was selected,the extraction was performed on 60 ℃ for 25 minutes,the concentration of salting-out agent NaCl was 20%.In chromatographic process,Agilent DB-5MS column(60 m×0.25 mm×1.00 μm)was applied for component separation.2-isobutyl-3-methoxypyrazine was chosen to be internal standard.The MDLS of 22-DMD,cis-2-EMD,trans-2-EMD,2E2MD,2-EDD were 1.6,0.6,0.5,1.0,0.3 ng/L respectively.The RSDs of target compounds in parallel spiked samples of pure water,raw water,finished water and distribution system water were 1.6%to 8.6%,the recovery rates were 94%to 117%.The method characteristic indices all met the determination requirements of trace level of cyclic acetals compounds in water.

headspace SPMEcyclic acetalsodorous compoundstrace level analysisGC-MS

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上海城投原水有限公司,上海 200125

顶空固相微萃取 环状缩醛 嗅味物质 痕量分析 气质联用法

2024

净水技术
上海市净水技术学会,上海市城乡建设和交通委员会科学技术委员会办公室

净水技术

CSTPCD
影响因子:0.643
ISSN:1009-0177
年,卷(期):2024.43(3)
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