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作 者:李碧波 杜鹏程 裴娟娟 LI Bibo;DU Pengcheng;PEI Juanjuan(Xiantao Inspection and Testing Center,Xiantao 433000)
出 处:《食品工业》2021年第3期314-317,共4页The Food Industry
摘 要:为加强流通环节豆芽类样品监管,建立液相质谱联用系统(LC-MS/MS)测定豆芽菜中4-氯苯氧乙酸钠(4-CPA-Na)和6-苄基腺嘌呤(6-BA)含量的快速试验方法。豆芽样品加入乙酸乙腈剧烈振摇后,超声提取,加入氯化钠、无水硫酸镁、C18粉末脱水净化。用空白基质提取液稀释后即可进入液相色谱,梯度程序洗脱后,通过质谱检测器分析,基质匹配外标法定量。4-CPA-Na和6-BA在0.1~20 ng/mL浓度区间内有良好线性关系(R^(2)≥99.9)。进行添加浓度1, 5和20μg/kg的加标回收率测试(n=5)。结果表明, 4-CPA-Na平均回收率87.2%~96.0%, RSD2.9%~4.5%,检出限0.4μg/kg,定量限1.0μg/kg;6-BA平均回收率89.2%~97.4%, RSD 2.6%~4.3%,检出限0.125μg/kg,定量限0.50μg/kg。该方法定性定量快速、稳定性高、再现性好,完全满足2种药物的检测分析。In order to strengthen the supervision of bean sprout samples in circulation, a high efficiency method was developed for the determination of 4-chlorophenoxyacetate(4-CPA-Na) and 6-benzyl Adenine(6-BA) in bean sprouts by liquid chromatography-tandem mass spectrometry(LC-MS/MS). The bean sprout sample was extracted by ultrasonic after acetonitrile acetate was added and shaken violently, dehydrated and purified by sodium chloride, anhydrous magnesium sulfate and C18 powder. After dilution with blank Matrix extract, it could be entered into liquid chromatography, eluted by gradient program, analyzed by mass spectrometer, Matrix matching external standard method for quantitative analysis. The 4-CPA-Na and 6-BA had good linear relationship in the concentration range of 0.1-20 ng/mL(R^(2)≥99.9). The addition concentrations of 1, 5 and 20 μg/kg standard recovery test(n=5) showed that the recovery rate of 4-CPA-Na was 87.2%-96.0%, and the relative standard deviation was 2.9%-4.5%;Detection limit was 0.4 μg/kg and quantitative limit was 1.0 μg/kg;The recovery rate of 6-BA was 89.2%-97.4%, and the relative standard deviation was 2.6%-4.3%;Detection limit was 0.125 μg/kg and quantitative limit was 0.5 μg/kg. The method was simple, rapid, sensitive and reproducible, and could be used for the determination of two drugs.
关 键 词:液相质谱联用系统(LC-MS/MS) 4-氯苯氧乙酸钠 6-苄基腺嘌呤 豆芽
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