GC-MS/MS Determination of 16 Phthalate Esters and 2 Monoester Metabolites of Phthalate Esters in Soil
摘 要
土壤样品经丙酮与正己烷以体积比1∶2组成的混合液提取,采用PSA/Silica复合填料玻璃柱净化,收集洗脱液,洗脱液旋蒸近干,加入正己烷,采用气相色谱-串联质谱法测定稀释液中16种邻苯二甲酸酯(PAEs)的含量。在气相色谱分离中采用DB-5MS石英毛细管色谱柱,在串联质谱分析中采用选择离子监测模式。测定2种邻苯二甲酸酯单酯代谢物(MPEs)时,洗脱液旋蒸近干后,在14%(质量分数)三氟化硼-甲醇溶液中于60℃衍生30 min。16种PAEs的线性范围均为0.02~0.80 mg·L-1,检出限(3S/N)为1.357 μg·kg-1;2种MPEs的线性范围均为0.05~1.00 mg·L-1,检出限(3S/N)为0.217 μg·kg-1。以空白土壤样品为基体进行加标回收试验,所得回收率为71.1%~105%,测定值的相对标准偏差(n=5)为0.10%~14%。
Abstract
The soil sample was extracted with the mixture of acetone and n-hexane (volume ratio of 1∶2). After purification with PSA/Silica composite packing glass column, the eluent was collected, and then evaporated to near dryness by rotary. After adding n-hexane, GC-MS/MS was applied to the determination of 16 phthalate esters (PAEs) in the diluent. The DB-5MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS/MS determination. For determination of 2 monoester metabolites of phthalate esters (MPEs), the eluent was evaporated to near dryness by rotary,and then derivatized for 30 min with mixture of boron trifluoride (14%, mass fraction) and methanol at 60 ℃. Linearity ranges of the 16 PAEs were found in the same range of 0.02-0.80 mg·L-1 with detection limits (3S/N) of 1.357 μg·kg-1. Linearity ranges of the 2 MPEs were found in the same range of 0.05-1.00 mg·L-1 with detection limits (3S/N) in the range of 0.217 μg·kg-1. On the base of blank soil sample, test for recovery was made by standard addition method; values of recovery found were in the range of 71.1%-105%, with RSDs (n=5) of determined values in the range of 0.10%-14%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202007011
所属栏目 专题报道(环境分析)
基金项目 中国热带农业科学院基本科研业务费专项资金(1630082019005);海南省重点研发计划(ZDYF2019131)
收稿日期 2020/3/6
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备注王晓燕,硕士研究生,主要从事有机污染物的分析与检测工作
引用该论文: WANG Xiaoyan,HUAN Zhibo. GC-MS/MS Determination of 16 Phthalate Esters and 2 Monoester Metabolites of Phthalate Esters in Soil[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(7): 799~803
王晓燕,郇志博. 气相色谱-串联质谱法测定土壤中16种邻苯二甲酸酯和2种邻苯二甲酸酯单酯代谢物[J]. 理化检验-化学分册, 2020, 56(7): 799~803
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