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采用溶剂萃取分离提取水样中的6种邻苯二甲酸酯(PAEs)代谢物邻苯二甲酸单丁酯、邻苯二甲酸单乙基己基酯、邻苯二甲酸、原儿茶酸、苯甲酸和邻苯二酚，优化了提取步骤和仪器检测参数，建立了简便、快速测定水样中6种PAEs代谢物的高效液相色谱法。结果表明，样品酸化是提高亲水性PAEs代谢物回收率的关键，添加终浓度为0.5%(V/V)的盐酸，6种PAEs代谢物的平均回收率为80.4%～101.6%。选择流动相为乙腈-0.3%甲酸(60∶40,V/V)进行等度洗脱，优化色谱条件下，6种PAEs代谢物在0.1～20 mg/L范围内线性关系良好(R2>0.9971),检出限(LODs)为4.5～10.8μg/L。以无机盐培养基为供试水样，在3个加标水平下，6种PAEs代谢物在水样中的平均加标回收率为79.9%～105%,相对标准偏差均小于5%,该方法适用于水环境中PAEs代谢物含量监测。将方法应用于枯草芽孢杆菌W34对邻苯二甲酸二正丁酯的代谢途径分析，发现该菌可将其快速水解为邻苯二甲酸单丁酯，但不能进一步代谢邻苯二甲酸单丁酯。
Abstract：Herein, we developed a simple and efficient method for the simultaneous extraction and determination of six phthalic acid esters(PAEs) metabolites(i.e.,mono-butyl phthalate(MBP),mono-(2-ethylhexyl) phthalate(MEHP),phthalic acid(PA),protocatechuic acid(PCA),benzoic acid(BA),and catechol(CT)) in water using liquid–liquid extraction techniques, followed by high performance liquid chromatography(HPLC) detection.The results indicated that sample acidification significantly influences the recovery of hydrophilic metabolites, with the addition of 0.5%(V/V) hydrochloric acid achieving average recoveries ranging from 80.4% to 101.6% for spiked water samples.In addition, chromatographic conditions were optimized using isocratic elution with a mobile phase of acetonitrile-0.3% formic acid(60∶40,V/V),a flow rate of 1.0 mL/min, an injection volume of 10 μL,a determined wavelength range of 190-280 nm, and a column temperature of 25 ℃.Under these optimal conditions, good linearity(R2 value>0.9971) was observed at concentration range of 0.1-20 mg/L,and the limits of detection(LODs) were 4.5-10.8 μg/L for the 6 metabolites in the water matrix.To validate the method, minimal salt medium(MSM) was spiked with the target metabolites at three concentration levels.The average recoveries ranged from 79.9% to 105%,with relative standard deviations(RSDs) below 5%,confirming the accuracy and precision of the method.This method is suitable for monitoring PAE metabolites in water samples.Furthermore, the method was successfully used to investigate the metabolic pathway of di-n-butylphthalate(DBP) in Bacillus subtilis strain W34.The results indicated that the strain rapidly hydrolyzed DBP to MBP,but MBP was not further metabolized.
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基本信息:
DOI：10.13526/j.issn.1006-6144.2024.12022
中图分类号:X832;O657.72
引用信息:
[1]王亚,郭秋晨,陈思棋,等.高效液相色谱法同时测定水样中的6种邻苯二甲酸酯代谢物[J].分析科学学报,2025,41(05):516-522.DOI:10.13526/j.issn.1006-6144.2024.12022.
基金信息:
国家自然科学基金(32272600); 江苏省农业科技自主创新资金(CX(22)2036)