文章摘要
陈丽香1,2,3 ,许佩勤1,2*.气相色谱-质谱联用仪测定柑橘类水果中2,4-滴的 残留量[J].海南师范大学学报自科版,2023,36(4):429-434
气相色谱-质谱联用仪测定柑橘类水果中2,4-滴的 残留量
Determination of 2,4-D Residues in Citrus Fruits by Gas Chromatography-mass Spectrometry
  
DOI:10.12051/j.issn.1674-4942.2023.04.011
中文关键词: 2,4-滴  气相色谱-质谱联用仪  柑橘类水果
英文关键词: 2,4-D  gas chromatography-mass spectrometry instrument  citrus fruit
基金项目:广东省工程技术研究中心平台建设项目(粤科函产字〔2020〕141号);广州市创新环境计划项目(2021-00-01- 13-5007-0001)
作者单位
陈丽香1,2,3 ,许佩勤1,2* 1.广东省食品工业公共实验室广东 广州 511442 2.广东省食品工业研究所有限公司广东 广州 511442 3.广东省食品质量监督检验站广东 广州 511442 
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中文摘要:
      建立一种用气相色谱质谱联用仪(GC-MS)测定柑橘类水果中2,4-滴残留量的方法。 在酸性条件下采用乙醚提取,硫酸作为催化剂,用正丁醇将2,4-滴衍生成2,4-滴丁酯,使用气相色 谱-质谱联用仪测定柑橘中2,4-滴的残留量(外标法定量)。结果表明,2,4-滴在0~0.5 µg/mL范 围内线性良好,相关系数(R2 )大于0.999,方法检出限为0.002 5 mg/kg,定量限为0.005 mg/kg。对沃 柑分别添加 0.005、0.01 和 0.1 mg/kg 3 个水平的 2,4-滴进行加标回收试验,回收率为 86.61%~ 99.32%,相对标准偏差为2.08%~4.46%(n = 6)。该方法灵敏度高,回收率稳定,定性定量准确,适 用于柑橘类水果中2,4-滴的测定。
英文摘要:
      To develop a method for the determination of 2,4-D residues in citrus fruits by gas chromatography-mass spec⁃ trometry (GC-MS), 2,4-D was extracted with diethyl ether under acidic conditions, and derived into 2,4-D butylate by nbutanol with sulfuric acid as catalyst. The residual amount of 2,4-D in citrus was determined by gas chromatography-mass spectrometry and quantified by external standard method. The results showed that 2,4-D had a good linearity in the range of 0-0.5 µg/mL, and the correlation coefficient (R2 ) was greater than 0.999. The detection limit and quantitation limit of the method were 0.002 5 mg/kg and 0.005 mg/kg respectively. The recoveries ranged of the 2,4-D were between 86.61% to 99.32% when 0.005 mg/kg, 0.01 mg/kg and 0.1 mg/kg of 2,4-D were added to citrus. Meanwhile, the relative standard devi⁃ ations (RSDs) were 2.08% to 4.46% (n = 6). The method had high sensitivity, stable recovery rate, accurate qualitative and quantitative analysis, and was suitable for the determination of 2,4-D in citrus fruits.
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