超高效液相色谱法测定贻贝中苯和二甲苯的代谢物

Determination of the Metabolites of Benzene and Xylene in Mussel by Ultra Performance Liquid Chromatography

[目的]建立二极管阵列检测器-超高效液相色谱(PDA-UPLC)法检测贻贝中苯和二甲苯代谢物的方法。[方法]贻贝样品经盐酸水解,乙酸乙酯提取,正己烷净化,以15 mmol/L乙酸铵-甲醇为流动相,检测波长为235 nm,流速0.2 mL/min, Waters ACQUITY UPLC■ BEH C_(18)柱分离,外标法定量。[结果]苯和二甲苯代谢物在各自线性范围内呈良好的线性关系(R^(2)>0.99),方法检出限为10.0~25.0μg/kg,定量限为20.0~50.0μg/kg,平均回收率在83.40%~113.10%,相对标准偏差(RSD)不大于8.62%。[结论]该方法具有操作简单、准确定性和灵敏度较高的特点,适合贻贝中苯和二甲苯代谢物残留量的测定。

[Objective]To establish a method for the detection of benzene and xylene metabolites in mussels by photodiode array detector-ultra performance liquid chromatography(PDA-UPLC).[Method] Mussel samples were hydrolyzed by hydrochloric acid, extracted with ethyl acetate, purified with n-hexane, then identification and quantification of the concentrate was carried out under the wavelength of 235 nm with the mobile phase consisted of 15 mmol/L ammonium acetate water-methanol at the flow rate of 0.2 mL/min and separated on a Waters ACQUITY UPLC■ BEH C_(18) column using external standard method. [Result]Benzene and xylene metabolites showed a good linear relationship within their respective linear ranges(R^(2)>0.99).The detection limit of the method was 10.0-25.0 μg/kg, the quantification limit was 20.0-50.0 μg/kg, the average recovery was 83.40%-113.10%, and the relative standard deviation(RSD) was not more than 8.62%.[Conclusion]The method has the characteristics of simple operation, accurate quality and high sensitivity, and is suitable for the determination of benzene and xylene metabolite residues in mussels.