QuEChERS-高效液相色譜-串聯(lián)質(zhì)譜法測定植物源食品中環(huán)磺酮殘留
發(fā)布時間:2018-03-29 16:08
本文選題:環(huán)磺酮 切入點:植物源食品 出處:《分析化學(xué)》2017年01期
【摘要】:建立了高效液相色譜-串聯(lián)質(zhì)譜法(HPLC-MS/MS)測定植物源食品中環(huán)磺酮殘留量的分析方法。樣品經(jīng)改進的Qu ECh ERS方法一步完成萃取凈化,經(jīng)酸化乙腈(含0.1%(V/V)甲酸的乙腈)提取,經(jīng)石墨化碳黑(GCB)凈化,提取液經(jīng)離心后直接過膜上機檢測。HPLC-MS/MS方法以0.1%(V/V)甲酸-乙腈為流動相,在0.25 m L/min流速下梯度洗脫,采用C18色譜柱進行液相色譜分離,電噴霧正離子電離(ESI+),多重反應(yīng)監(jiān)測模式(MRM)檢測,基質(zhì)匹配外標(biāo)法進行定量分析。結(jié)果表明,在10種基質(zhì)(玉米、大米、小麥、葡萄、蘋果、葡萄干、枸杞、西紅柿、黃瓜、白菜)中,環(huán)磺酮在0.5~100.0 ng/m L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)均大于0.996;方法定量限(S/N≥10)為1.0μg/kg;在1.0,2.0和10.0μg/kg添加水平下,環(huán)磺酮的平均回收率為82.0%~111.8%,相對標(biāo)準(zhǔn)偏差為3.0%~14.9%。本方法高效快捷,靈敏度、準(zhǔn)確度和精密度均符合農(nóng)藥殘留檢測要求。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was established for the determination of the residues of cyclosulfonone in vegetable foods. The samples were extracted and purified by an improved qu ECh ERS method. The samples were extracted by acidified acetonitrile (acetonitrile containing 0.1 V / V) formic acid. After purification by graphitized carbon black (L/min), the extract was separated by liquid chromatography on C18 column after centrifugation. The mobile phase was 0.1 V / V form-acetonitrile, the mobile phase was 0.1 V / V formic acid-acetonitrile, and the separation was carried out on a C18 chromatographic column with a gradient elution at a flow rate of 0.25 m L/min. Electrospray positive ion ionization (ESI), multiple reaction monitoring model (MRM), matrix matching external standard method were used for quantitative analysis. The results showed that, in 10 substrates (corn, rice, wheat, grape, apple, raisin, medlar, tomato, cucumber), In Chinese cabbage, the linear range of cyclosulfonone was 0.5 ~ 100.0 ng/m / L, the correlation coefficients were all greater than 0.996; the quantification limit S / N 鈮,
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