超高效液相色谱-串联质谱法同时分析地下水中24种内分泌干扰物

Simultaneous Analysis of 24 Endocrine Disruptors in Groundwater by Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry

建立了基于超高效液相色谱-串联质谱法同时测定地下水中9种雌激素、5种雄激素、3种肾上腺皮质激素、4种酚类和3种非甾类激素共24种内分泌干扰物的方法。在活化后的MCX固相萃取柱中加入水样,再加入pH=5的水溶液淋洗,随后用碱化乙腈(4.5%,体积分数)洗脱。收集洗脱液并用氮气吹至近干后,用甲醇定容。采用Poroshell 120 Bonus-RP色谱柱(2.7μm,100 mm×2.1 mm),以0.1%氨水溶液-乙腈为流动相进行梯度洗脱,实现液相分离。质谱检测采用MRM模式进行采集,通过正负离子模式切换同时进行测定,使用内标法定量。检测结果显示,目标物在线性范围内,决定系数R2均大于0.995,方法检出限为0.05~2.00 ng/L,加标回收率为68.8%~108%。该方法灵敏度高、准确度好,具有较强的实用价值。

A method for simultaneous determination of 24 endocrine disruptors(9 estrogens,5 androgens,3 adrenocortical hormones,4 phenols and 3 nonsteroidal hormones)in groundwater by ultra-performance liquid chromatography tandem mass spectrometry was established.Water samples were added to the activated MCX solid-phase extraction column,and then aqueous solution with pH=5 was added for washing,followed by elution with alkalized acetonitrile(4.5%,V/V).The collected eluent was blown to near-dry with nitrogen and methanol was constant volumed.The separation was performed on an Poroshell 120 Bonus-RP(2.7μm,100 mm×2.1 mm)column with a gradient elution of 0.1%ammonia aqueous solution-acetonitrile mobile phase.Mass spectrometry was performed by MRM mode.The positive and negative ion modes were switched for simultaneous determination,quantification by internal standard method.The results showed that the target compounds was in the linear range,the determination coefficient R2 were greater than 0.995,the detection limit was between 0.05 and 2.00 ng/L,and the recoveries were between 68.8%and 108%.The developed method showed high sensitivity,good accuracy as well as strong practical value in the future.