全自动固相萃取-超高效液相色谱-三重四级杆质谱法测定水中4种卤代苯醌

Determination of 4 halobenzoquinones in water by fully automatic solid phase extraction ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry

目的建立水中2.6-二氯-1.4苯醌、2.5-二溴-1.4苯醌、2.3.5.6-四溴-1.4苯醌和3.4.5.6-四氯-1,2苯醌的全自动固相萃取-超高效液相色谱-三重四级杆质谱法快速测定方法。方法采用全自动固相萃取法,水样上样体积200ml,经HLB固相萃取柱净化、以0.1%甲酸-甲醇溶液洗脱。洗脱液以BEH C_(18)色谱柱为分离柱,甲醇和0.1%甲酸水溶液为流动性,在电喷雾负离子多反应监测(MRM)模式下检测,外标法定量。结果4种卤代苯醌在0.25ng/L~100ng/L内所有化合物响应因子的RSD均在10%以内,且呈良好的线性关系,相关系数>0.9990,方法检出限为0.1ng/L~0.3ng/L。对添加高、中、低3个浓度水平的水样分别进行6次平行分析,平均回收率为81.3%~113.4%,相对标准偏差为1.5%~4.3%(n=6)。结论本方法简单、快速,灵敏度高,能满足水中卤代苯醌测定的要求。

Objective To establish a method for the simultaneous detection of four halobenzoquinones including 2,6-dichloro-1,4-benzoquinone,2-dibromo-1,2-dibromo-1,2-benzoquinone,2-tetrabromo-1,4-benzoquinone and 3-tetrabromo-1,2-benzoquinone in water by fully automatic solid phase extraction-ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry.Methods The water samples were purified by HLB solid phase extraction column and eluted with 0.1%formic acid and methanol solution.Then the eluants were separated with a BEH C_(18) column using a gradient program with methanol-0.1%formic acid aqueous as the mobile phase,and detected by negative electro-spray ionization tandem mass spectrometer in the MRM mode,and quantified by standard curves.Results The method was linear in the range of 0.25 ng/L-100 ng/L,and theRSDof the response factors were within 10%.The correlation coefficient was higher than 0.999 0,and the detection limit was within 0.1 ng/L-0.3 ng/L.The average recoveries were within 81.3%-113.4%,and the relative standard deviations (RSDs) were within 1.5%-4.3%(n=6).Conclusion The method is simple,rapid and sensitive,and it can be applied for determination of four halobenzoquinones in water.