發(fā)布時(shí)間：2018-02-24 16:06

  本文關(guān)鍵詞： 百草枯 二維液相色譜法 尿液 自動(dòng)化　出處：《中國(guó)藥學(xué)雜志》2017年10期 　論文類(lèi)型：期刊論文

【摘要】：目的采用新型二維液相色譜系統(tǒng)(2D-LC-UV)建立中毒患者尿液中百草枯濃度的測(cè)定方法,并對(duì)二維色譜特征及方法學(xué)進(jìn)行評(píng)估。方法 2D-LC-UV由第一維和第二維液相色譜系統(tǒng)及FLC轉(zhuǎn)運(yùn)機(jī)構(gòu)構(gòu)成,尿液100μL直接進(jìn)樣,在第一維Aston SX1色譜柱(4.6 mm×250 mm,5μm)上進(jìn)行在線富集及初級(jí)分離,通過(guò)Aston SX捕集柱(4.6 mm×100 mm,5μm)捕集保留,最后轉(zhuǎn)移到第二維色譜柱Aston SX1(4.6 mm×75 mm,5μm)上進(jìn)一步分離檢測(cè)。第一維流動(dòng)相為2 mol·L~(-1)醋酸銨-乙腈=10∶1(V∶V),流速1.0 mL·min~(-1),捕集柱流動(dòng)相為純水,第二維流動(dòng)相為2.5 mol·L~(-1)醋酸銨-甲醇-乙腈=5∶3∶1(V∶V∶V),流速1.0 mL·min~(-1),柱溫40℃,紫外檢測(cè)波長(zhǎng)285 nm。結(jié)果所建立的二維色譜方法可以去除樣品中大部分雜質(zhì),最大可以在線處理500μL樣品,目標(biāo)物在二維系統(tǒng)中轉(zhuǎn)移完整;在20~20 000ng·mL~(-1)內(nèi)線性關(guān)系良好(r=0.999 9),不同來(lái)源尿液中未發(fā)現(xiàn)干擾;工作曲線可長(zhǎng)時(shí)間穩(wěn)定,色譜平衡時(shí)間小于15min。結(jié)論本方法穩(wěn)定性良好、簡(jiǎn)便快速、結(jié)果準(zhǔn)確、自動(dòng)化程度高,不依賴(lài)于專(zhuān)門(mén)的技術(shù)人員,適用于臨床百草枯中毒患者的快速檢測(cè),為臨床制定解救方案提供科學(xué)依據(jù)。
[Abstract]:Objective to establish a new two-dimensional liquid chromatographic system, 2D-LC-UV, for the determination of paraquat concentration in urine of poisoning patients. Methods 2D-LC-UV was composed of first and second dimensional liquid chromatography system and FLC transporter. Urine was directly injected with 100 渭 L urine. The sample was preenriched on the first dimensional Aston SX1 column (4.6 mm 脳 250mm / 5 渭 m), and the primary separation was performed on the first dimensional Aston SX1 chromatographic column (4.6mm 脳 250mm / 5 渭 m). Aston SX trapping column (4.6mm 脳 100mm-1 渭 m) was used for further separation and detection. The mobile phase was 2 mol 路L ~ (-1) acetonitrile (10: 1) with a flow rate of 1.0 mL 路min ~ (-1) 路min ~ (-1). The mobile phase of the column was pure water, and the flow rate was 1.0 mL 路min ~ (-1) 路min ~ (-1). The second mobile phase is 2.5 mol 路L ~ (-1)) ammonium acetate, methanol-acetonitrile, 5: 3: 1: 1: v: v: v, flow rate 1.0 mL 路min ~ (-1), column temperature 40 鈩，

本文編號(hào)：1530854