| 气相色谱-串联质谱法测定豆乳中12 种有机磷及氨基甲酸酯类农药残留 |
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| 引用本文： | 谢瑞龙,梁建英.气相色谱-串联质谱法测定豆乳中12 种有机磷及氨基甲酸酯类农药残留[J].乳业科学与技术,2021,44(5):27-31. |
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| 作者姓名： | 谢瑞龙 梁建英 |
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| 作者单位： | （内蒙古伊利实业集团股份有限公司，内蒙古 呼和浩特 010110） |
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| 摘 要： | 建立QuEChERS-气相色谱-串联质谱法测定豆乳中12 种有机磷及氨基甲酸酯类农药残留的方法。样品经乙腈提取，柠檬酸盐缓冲条件下分离，无水硫酸镁、乙二胺-N-丙基硅烷化硅胶和C18净化处理，气相色谱-串联质谱仪测定。结果表明：12 种农药的定量限均为0.004 mg/kg；标准曲线在5～200 ng/mL范围内线性良好，相关系数＞0.99；进行3 个不同水平的加标实验，加标回收率为71.8%～114.9%，相对标准偏差为4.6%～13.3%。该方法快速、高效、准确，可用于豆乳中有机磷及氨基甲酸酯类农药残留的测定。
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| 关 键 词： | QuEChERS 气相色谱-串联质谱 豆乳 有机磷 氨基甲酸酯 |
Determination of 12 Organophosphorus and Carbamate Pesticide Residues in Soy Milk by Gas Chromatography-Tandem Mass Spectrometry |
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| XIE Ruilong,LIANG Jianying.Determination of 12 Organophosphorus and Carbamate Pesticide Residues in Soy Milk by Gas Chromatography-Tandem Mass Spectrometry[J].JOURNAL OF DAIRY SCIENCE AND TECHNOLOGY,2021,44(5):27-31. |
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| Authors: | XIE Ruilong LIANG Jianying |
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| Institution: | (Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 010110, China) |
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| Abstract: | A method based on quick, easy, cheap, effective, rugged, safe (QuEChERS) extraction combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the simultaneous quantitative determination of 12 organophosphorus and carbamate pesticide residues in soy milk. The samples were extracted with acetonitrile, then the supernatant was separated after addition of citrate buffer, followed by cleanup with a mixture of anhydrous magnesium sulfate, primary secondary amine (PSA) and C18 sorbents. The analytes were detected by GC-MS/MS. The results showed that the limits of quantification (LOQs) were 0.004 mg/kg for the 12 pesticides. The calibration curves were linear in the concentration range of 5–200 ng/mL with correlation coefficient greater than 0.99. The recoveries varied from 71.8% to 114.9% with relative standard deviation (RSD) from 4.6% to 13.3% at three different spiked levels. The method was found to be quick, efficient, accurate and suitable for the determination of organophosphorus and carbamate pesticide residues in soy milk. |
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| Keywords: | quick easy cheap effective rugged safe gas chromatography-tandem mass spectrometry soy milk organophosphorus carbamate |
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