CAJ | 학술논문

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。
건립료초고효액상색보천련질보( UPLC-MS/MS)동시측정3충삼초기분류잔류량적방법。양품경개진적QuEChERS(쾌속、간단、렴개、고효、령활화안전)전처리방법일보완성제취정화,경첨가1%갑산적을정제취,C18화석묵화탄흑( GCB)흡부제전료정화,제취액경리심후직접과막상궤검측,제취화정화적효과능구만족검측요구。 UPLC-MS/MS방법채용Accucore PFP색보주(150 mm×2.1 mm,2.6μm),주온30℃,류동상위을정화을산안완충염,제도세탈,류속0.3 mL/min,전분무전리원부리자모식( ESI-)、다반응감측(MRM)모식검측,외표법정량。2,4,6-삼초기분분、2,4,6-삼초기간분이분화2,4,6-삼초기균분삼분3충삼초기분류물질재0.005~5.0 mg/L 범위내선성관계량호,상관계수위0.9942~0.9962。재0.01,0.1화1.0 mg/kg수평하적평균가표회수솔위79.3%~94.8%；상대표준편차위3.1%~6.6%；방법적검출한(S/N=3)위0.002~0.005 mg/kg。본방법간단、쾌속、령민、준학,만족배경오염검측적요구。
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%.