本文選題：氣相色譜-質(zhì)譜　切入點(diǎn)：QuEChERS　出處：《色譜》2017年12期

【摘要】：建立了QuEChERS-氣相色譜-質(zhì)譜同時(shí)測定土壤中乙草胺(acetochlor)、甲草胺(alachlor)、異丙甲草胺(metolachlor)、吡草胺(metazachlor)、丁草胺(butachlor)和丙草胺(pretilachlor)6種酰胺類除草劑的分析方法。土壤中殘留的酰胺類除草劑用10 mL去離子水、10 mL乙腈和4 g NaCl提取,用N-丙基乙二胺(PSA)、C18、石墨化炭黑(GCB)和無水硫酸鎂(MgSO4)凈化,然后用氣相色譜-質(zhì)譜聯(lián)用法測定。采用HP-5MS弱極性石英毛細(xì)管柱進(jìn)行氣相色譜分離,在電子轟擊電離(EI)源模式下以選擇離子監(jiān)測(SIM)掃描模式檢測。結(jié)果表明,6種酰胺類除草劑在0.01~1.00 mg/L范圍內(nèi)呈良好線性關(guān)系,相關(guān)系數(shù)(r)為0.999 6~1.000 0。在加標(biāo)水平為0.025、0.10和0.50 mg/kg時(shí),6種酰胺類除草劑的平均回收率為92.0%~108%,相對標(biāo)準(zhǔn)偏差為1.64%~8.25%(n=3)。方法的檢出限為0.002~0.006 mg/kg,定量限為0.005~0.02 mg/kg。同常用的氣相色譜-電子捕獲檢測(GC-ECD)法比較,該法可提高抗干擾能力,使6種酰胺類除草劑得到較好分離。方法所使用的有機(jī)溶劑種類和用量少,操作簡單、快速,具有應(yīng)用價(jià)值。
[Abstract]:A method was established for simultaneous determination of Acetochlor, alachlora, metolachloror, pyramidine, butachloror, butachloror and promethylamine in soil by QuEChERS- gas chromatography-mass spectrometry. Residues of amides in soil. 10 mL deionized water was extracted with 10 mL acetonitrile and 4 g NaCl. N- propyl ethylenediamine (PSAA) C18, graphitized carbon black (GCBB) and anhydrous magnesium sulfate (MgSO4) were purified and determined by gas chromatography-mass spectrometry. HP-5MS capillary column with weak polarity was used for gas chromatographic separation. In the mode of electron bombardment ionization ionization ionization (ei) source, the selective ion monitoring (SIM) scanning mode was used to detect the herbicides. The results showed that there was a good linear relationship between the six kinds of herbicides in the range of 0.01 ~ 1.00 mg/L. The correlation coefficient (r) is 0.999 ~ 1.0000.The average recovery rate of the six kinds of amide herbicides is 92.0 ~ 108.The relative standard deviation is 1.64 ~ 8.25g / kg, the detection limit is 0.0020.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg. The average recovery rate of six kinds of amide herbicides is 92.0 ~ 108g / kg. The detection limit is 0.0020.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg / g. The relative standard deviation is 1.64% ~ 8.25mg / kg. The detection limit of the method is 0.002 0.006 mg / kg and the quantitative limit is 0.0050.02 mg / kg. Comparison of capture detection with GC-ECD, The method can improve the anti-interference ability and make 6 kinds of amide herbicides better separated. The method uses less organic solvents and amounts of organic solvents, and is easy to operate, fast, and has application value.
【作者單位】： 云南省農(nóng)業(yè)科學(xué)院質(zhì)量標(biāo)準(zhǔn)與檢測技術(shù)研究所農(nóng)業(yè)部農(nóng)產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)測試中心;
【基金】：云南省科技創(chuàng)新平臺建設(shè)計(jì)劃項(xiàng)目(2014DA001) 云南省創(chuàng)新團(tuán)隊(duì)計(jì)劃項(xiàng)目(2015HC025)~~
【分類號】：O657.63;X833

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本文編號：1699434