發(fā)布時(shí)間：2018-06-21 15:47

  本文選題：高效液相色譜-串聯(lián)質(zhì)譜法 + 薄膜微萃取��； 參考：《理化檢驗(yàn)(化學(xué)分冊(cè))》2016年12期

【摘要】：取樣品1.00mL與正己烷9.00mL混勻,加入1mol·L-1氫氧化鈉溶液10μL,于此溶液投入濾紙條,并振蕩120min。取出濾紙條,用正己烷蕩洗2次去油后,用乙腈-鹽酸(100+1)混合液1.00mL洗脫,分出洗出液;濾紙用甲醇1.0mL洗滌,洗液與洗出液合并后進(jìn)行色譜分離。以ACQUITY UPLC BEH C18色譜柱為分離柱,以不同體積比的甲醇和0.1%(體積分?jǐn)?shù))甲酸溶液的混合液為流動(dòng)相進(jìn)行梯度洗脫。在質(zhì)譜分析中采用電噴霧正離子源和多反應(yīng)監(jiān)測(cè)模式檢測(cè)。4-硝基酚(4-NP)和2,4-二硝基酚(2,4-DNP)的質(zhì)量濃度均在10~1 000μg·L-1內(nèi)與其峰面積呈線性關(guān)系,4-NP及2,4-DNP的檢出限(3s)分別為2.5,3.0μg·L-1。加標(biāo)回收率在81.3%~97.8%之間,測(cè)定值的相對(duì)標(biāo)準(zhǔn)偏差(n=6)在1.6%~3.5%之間。
[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%.
【作者單位】： 徐州工業(yè)職業(yè)技術(shù)學(xué)院;徐州市產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)中心;
【分類(lèi)號(hào)】：X836;O657.63

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