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 |
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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) |
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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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