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表面活性剂辅助微萃取-高效液相色谱法测定尿中一氯苯的2种代谢物
          
HPLC Determination of 2 Metabolites of Monochlorobenzene in Urine with Surfactant Assisted Microextraction

摘    要
尿样以十六烷基三甲基溴化铵为辅助剂,正辛醇为萃取剂,萃取液离心后,取上层有机相,采用高效液相色谱法测定其中一氯苯的2种代谢物(4-氯邻苯二酚和对氯苯酚)的含量。以RD-C18色谱柱为分离柱,以甲醇与0.15%(体积分数)的磷酸溶液以体积比65:35组成的混合液为流动相,在检测波长280 nm处进行测定。4-氯邻苯二酚和对氯苯酚的质量浓度均在600 μg·L-1以内与其对应的峰面积呈线性关系,检出限(3S/N)为1.67,2.23 μg·L-1,测定下限(10S/N)为5.55,7.43 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为89.2%~97.4%,测定值的日内相对标准偏差(n=6)为2.1%~4.9%,日间相对标准偏差(n=18)为2.5%~5.3%。
标    签 高效液相色谱法   表面活性剂   微萃取   一氯苯   4-氯邻苯二酚   对氯苯酚   HPLC   surfactant   microextraction   monochlorobenzene   4-chlorocatechol   p-chlorophenol  
 
Abstract
The urine sample was extracted with n-octanol with hexadecyl trimethyl ammonium bromide as auxiliary solvent. The extract was centrifugated, and then the upper organic phase was taken. HPLC was applied to the determination of 2 metabolites (4-chlorocatechol and p-chlorophenol) of monochlorobenzene in the upper organic phase. RD-C18 chromatographic column was used as separation column, and a mixture of methanol and 0.15% (φ) phosphoric acid solution with volume ratio of 65∶35 was used as mobile phase. Detection at 280 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of 4-chlorocatechol and p-chlorophenol were kept in the same range within 600 μg·L-1, with detection limits (3S/N) of 1.67, 2.23 μg·L-1 and lower limits of determination (10S/N) of 5.55, 7.43 μg·L-1 respectively. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 89.2%-97.4%, with intra-day RSDs (n=6) and inter-day RSDs (n=18) of determined values in the ranges of 2.1%-4.9%, 2.5%-5.3%, respectively.

中图分类号 O652.63   DOI 10.11973/lhjy-hx202005004

 
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收稿日期 2019/10/9

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备注盛旭光,硕士研究生,研究方向为卫生检验与检疫

引用该论文: SHENG Xuguang,MEI Yong,NIE Menghan,CHEN Haichuan,WANG Gang. HPLC Determination of 2 Metabolites of Monochlorobenzene in Urine with Surfactant Assisted Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(5): 519~524
盛旭光,梅勇,聂梦涵,陈海川,王港. 表面活性剂辅助微萃取-高效液相色谱法测定尿中一氯苯的2种代谢物[J]. 理化检验-化学分册, 2020, 56(5): 519~524


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