氣相色譜-串聯(lián)質(zhì)譜法測(cè)定不同原產(chǎn)國(guó)抗草甘膦轉(zhuǎn)基因大豆中草甘膦及其代謝物的殘留量
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本文關(guān)鍵詞: 轉(zhuǎn)基因大豆 草甘膦 氨甲基膦酸 氣相色譜-串聯(lián)質(zhì)譜 出處:《食品安全質(zhì)量檢測(cè)學(xué)報(bào)》2016年09期 論文類型:期刊論文
【摘要】:目的利用氣相色譜-串聯(lián)質(zhì)譜(gas chromatography-tandemmass spectrometry,GC-MS/MS)法對(duì)防城港口岸進(jìn)境的不同原產(chǎn)國(guó)抗草甘膦轉(zhuǎn)基因大豆中的草甘膦及其代謝物-氨甲基膦酸的殘留量進(jìn)行檢測(cè),對(duì)比分析其差異。方法采集原產(chǎn)自美國(guó)、巴西、阿根廷和烏拉圭的抗草甘膦轉(zhuǎn)基因大豆各3批,樣品磨碎后過(guò)篩,用水提取,再用鹽酸沉淀蛋白,用二氯甲烷萃取脂肪,上層清液經(jīng)陽(yáng)離子交換柱(CAX柱)凈化后,再與七氟丁醇和三氟乙酸酐進(jìn)行衍生化反應(yīng),用檸檬醛-乙酸乙酯溶液定容,GC-MS/MS分析。結(jié)果草甘膦和氨甲基膦酸在2.5~100 ng/mL濃度范圍內(nèi)的質(zhì)量濃度與峰面積間的線性相關(guān)性較好(r0.999),檢出限均為0.05 mg/kg。樣品的加標(biāo)濃度為0.05、0.5和2.0 mg/kg時(shí)的平均回收率為77.1%~96.5%,相對(duì)標(biāo)準(zhǔn)偏差小于8.8%(n=6)。結(jié)論本方法的準(zhǔn)確度高、精密度良好,能滿足檢測(cè)工作的實(shí)際需求。
[Abstract]:Objective to detect glyphosate and its metabolite, aminomethylphosphonic acid, in glyphosate resistant soybean from different countries of origin in Fangchenggang port by gas chromatography-tandem mass spectrometry (gas chromatography-tandem mass spectrometry) method. Methods three batches of glyphosate resistant soybean were collected from USA, Brazil, Argentina and Uruguay. The samples were ground and sifted, extracted with water, then precipitated with hydrochloric acid, and extracted with dichloromethane. The supernatant was purified by cationic exchange column (CAX) and then reacted with heptafluorobutanol and trifluoroacetic anhydride. Results the linear correlation between the mass concentration of glyphosate and aminomethylphosphonic acid in the concentration range of 2.5 ~ 100 ng/mL was better than that of the peak area. The detection limit was 0. 05 mg / kg. The standard concentration of glyphosate and aminomethylphosphonic acid was 0. 05 mg / kg. The average recoveries at 0. 05 and 2. 0 mg/kg were 77. 1 and 96. 5, and the relative standard deviation was less than 8. 8%. Conclusion this method has high accuracy. Good precision, can meet the actual needs of the detection work.
【作者單位】: 防城港出入境檢驗(yàn)檢疫局;
【基金】:廣西出入境檢驗(yàn)檢疫局科技計(jì)劃項(xiàng)目(2015k011)~~
【分類號(hào)】:O657.63;TS207.53
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