滤纸薄膜微萃取-高效液相色谱-串联质谱法测定植物油中4-硝基酚和2,4-二硝基酚的含量

发布时间：2018-06-21 15:47

本文选题：高效液相色谱-串联质谱法 + 薄膜微萃取　；参考：《理化检验(化学分册)》2016年12期

【摘要】：取样品1.00mL与正己烷9.00mL混匀,加入1mol·L-1氢氧化钠溶液10μL,于此溶液投入滤纸条,并振荡120min。取出滤纸条,用正己烷荡洗2次去油后,用乙腈-盐酸(100+1)混合液1.00mL洗脱,分出洗出液;滤纸用甲醇1.0mL洗涤,洗液与洗出液合并后进行色谱分离。以ACQUITY UPLC BEH C18色谱柱为分离柱,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱。在质谱分析中采用电喷雾正离子源和多反应监测模式检测。4-硝基酚(4-NP)和2,4-二硝基酚(2,4-DNP)的质量浓度均在10~1 000μg·L-1内与其峰面积呈线性关系,4-NP及2,4-DNP的检出限(3s)分别为2.5,3.0μg·L-1。加标回收率在81.3%~97.8%之间,测定值的相对标准偏差(n=6)在1.6%~3.5%之间。
[Abstract]:Sample 1.00 mL was mixed with 9.00 mL of n-hexane, and 10 渭 L 1mol L-1 sodium hydroxide solution was added. The filter paper was put into the solution and oscillated for 120 min. The filter paper strip was removed, then washed with n-hexane for two times, then eluted with 1.00 mL acetonitrile-hydrochloric acid (1001) mixed solution, and then washed with methanol 1.0 mL, then separated by chromatography after the washing liquid was combined with the washing liquid. ACQUITY UPLC BEH C18 column was used as separation column and gradient elution was carried out with methanol of different volume ratio and mixture of 0.1 (volume fraction) formic acid solution as mobile phase. In mass spectrometric analysis, the detection limits of 4-nitrophenol 4-NPand 2-4-dinitrophenol 24-DNP) were linear with the peak area within 100.000 渭 g L-1 by electrospray ion source and multi-reaction monitoring mode. The detection limits of 4-NP and 2C4-DNP were 2.53.0 渭 g / L ~ (-1), respectively.The results showed that the detection limit was 2.53.0 渭 g / L ~ (-1) in the mass concentration range of 4- (4-NP) and 2-( 4-DNP) in the range of 10 ~ 1 000 渭 g 路L ~ (-1). The recoveries were between 81.3% and 97.8%, and the relative standard deviation (RSDs) was between 1.6% and 3.5%.
【作者单位】：徐州工业职业技术学院;徐州市产品质量监督检验中心;
【分类号】：X836;O657.63

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