QuEChERS-超高效液相色谱串联质谱法测定土壤中三硝基酚类物质  

QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry for Determination of 2,4,6-Trinitrophenol,2,4,6-trinitroresorcinate and 2,4,6-Trinitrophloroglucinol in Soil

作　　者：刘玉[1,2] 张同来[1] 杨利[1] 武碧栋[1] 刘芮[1] 

机构地区：[1]爆炸科学与技术国家重点实验室,北京理工大学,北京100081 [2]潍坊市食品药品检验检测中心,潍坊262500

出　　处：《分析化学》2014年第8期1183-1188,共6页Chinese Journal of Analytical Chemistry

基　　金：应用物理化学实验室科技基金(Nos.9140C3703051105;9140C370303120C37142);爆炸科学与技术国家重点实验室基金(No.QNKT12-02)资助项目

摘　　要：建立了超高效液相色谱串联质谱（UPLC-MS/MS）同时测定3种三硝基酚类残留量的方法。样品经改进的QuEChERS（快速、简单、廉价、高效、灵活和安全）前处理方法一步完成提取净化,经添加1%甲酸的乙腈提取,C18和石墨化炭黑（GCB）吸附剂填料净化,提取液经离心后直接过膜上机检测,提取和净化的效果能够满足检测要求。UPLC-MS/MS方法采用Accucore PFP色谱柱（150 mm×2.1 mm,2.6μm）,柱温30℃,流动相为乙腈和乙酸铵缓冲盐,梯度洗脱,流速0.3 mL/min,电喷雾电离源负离子模式（ESI-）、多反应监测（MRM）模式检测,外标法定量。2,4,6-三硝基苯酚、2,4,6-三硝基间苯二酚和2,4,6-三硝基均苯三酚3种三硝基酚类物质在0.005~5.0 mg/L范围内线性关系良好,相关系数为0.9942~0.9962。在0.01,0.1和1.0 mg/kg水平下的平均加标回收率为79.3%~94.8%;相对标准偏差为3.1%~6.6%;方法的检出限（S/N=3）为0.002~0.005 mg/kg。本方法简单、快速、灵敏、准确,满足环境污染检测的要求。A simple, rapid sensitive and accurate ultra performance liquid chromatography tandem mass spectrometric （ UPLC-MS/MS ） method was developed for the simultaneous determination of 2 , 4 , 6-trinitrophenol, trinitroresorcinate, trinitrophloroglucinol residues in soil. The sample was pretreated by using the modified QuEChERS （ quick, easy, cheap, effective, rigged, and safe ） method that completed the extraction and clean-up steps in one procedure. In this none buffer QuEChERS method, samples were extracted with 1% formic acid ﹢ acetonitrile, cleaned up with primary graphitized carbon black （ GCB） and C18 sorbent, then centrifuged and filtrated before detection. The pretreatment method was simple, rapid and effective and can meet the detection requirements. The UPLC-MS/MS method was performed on Waters Accucore PFP （150 mm× 2. 1 mm, 2. 6 μm） and the column temperature was 30 ℃, the gradient elution with acetonitrile and ammonium acetate as the mobile phase and the flow rate was 0. 3 mL/min. The negative electrospray ionization （ ESI-） source under the multiple reaction monitoring （ MRM ） mode and external standard method were used for quantification. The results showed that the correlation coefficients up to 0. 9942 were obtained across a concentration range of 0. 005-5. 0 mg/L. The limits of detection （ LOD） ranged from 0 . 002 to 0 . 005 mg/kg （ S/N=3 ） . The method was validated with soil samples spiked at three fortification levels （0. 01, 0. 1 and 1 mg/kg） and recoveries were in the range of 79. 3%-94. 8% with relative standard deviations （RSD） of 3. 1%-6. 6%.

关 键 词：超高效液相色谱串联质谱法 2 4 6-三硝基苯酚 2 4 6-三硝基间苯二酚 2 4 6-三硝基均苯三酚 QuEChERS方法 土壤 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]