高效液相色谱-三重四极杆串联质谱测定环境水样中20种环境内分泌干扰物
Determination of 20 endocrine-disrupting compounds in environmental water samples by high performance liquid chromatography-tandem mass spectrometry
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摘要: 环境内分泌干扰物（EDCs）是指干扰生物体内保持自身平衡和调节发育过程中天然激素的外源性化学物质.因EDCs对环境暴露生物体正常生长发育和繁殖带来的潜在危害，其已成为当前科学界和公众共同关注的热点问题之一.本论文建立了固相萃取-高效液相色谱-串联质谱测定水样中4类EDCs（孕激素、雄激素、雌激素和烷基酚）的分析方法.水样通过HLB小柱进行固相萃取和纯化，以甲醇和水为正模式流动相，孕激素和雄激素等物质在正模式下响应高；甲醇和0.1%氨水为负模式流动相，雌激素和烷基酚等物质在负模式下响应高.20种EDCs的定量分析通过三重四极杆串联质谱多反应监测模式分析.各目标物的检出限为0.04-0.51 ng·L-1，定量限为0.13-1.70 ng·L-1，回收率为76.1%-121.6%，相对标准偏差<15%.应用该方法对不同水体（河流水、湖泊水和生活污水）中EDCs的分布状况进行了初步调查，发现EDCs广泛存在于表层水样中，浓度范围为ND-981.1 ng·L-1.
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关键词:
- 水样 /
- 环境内分泌干扰物 /
- 高效液相色谱-三重四极杆串联质谱 /
- 固相萃取
Abstract: Endocrine-disrupting compounds (EDCs) are defined as exogenous agents that interfere with natural hormones in the body. EDCs have attracted a great deal of scientific and public attention worldwide due to their potential adverse effects on the normal reproduction and development of environmentally exposed organisms. An analytical method for 4 classes of EDCs (progesterone, testosterone, estrogen, alkylphenol) in water samples were developed with solid phase extraction-liquid chromatography-tandem mass spectrometry. Water sample was concentrated and cleaned up with HLB cartridge. Gradient elution was performed using methanol and 0.1% NH4OH, estrogen and alkylphenol were measured by negative ionization modes for sensitivity responses; methanol and water in positive ionization mode for estrogen and testosterone determination. The quantitative analysis of the targeted 20 EDCs was performed with the multiple reaction monitoring mode of triple quadruple tandem mass spectrometry. The limits of detection (LOD) and quantitation (LOQ) for the 20 EDCs were 0.04-0.51 ng·L-1 and 0.13-1.70 ng·L-1, respectively. The recoveries were in the range of 76.1%-121.6%, and the relative standard deviation <15%. This method was successfully applied to different water samples (river, lake and effluent) for analyzing the distribution of EDCs. The detection concentrations ranged from not detected to 981.1 ng·L-1 which reflected that EDCs might extensively exist in these surface water samples. -
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