GC Determination of Residual Amount of Ethephon in Grapes with Headspace
摘 要
称取葡萄样品于预先加入氯化钠的顶空瓶中,再加入饱和氢氧化钾溶液,采用顶空-气相色谱法测定上述混合液中乙烯利的残留量。顶空温度为75℃,顶空时间为90 min,采用HP-5色谱柱(30 m×0.32 mm,0.25 μm)分离,氢火焰离子化检测器测定。乙烯利的质量浓度在0.500~50.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.010 0 mg·kg-1。方法用于葡萄样品的分析,加标回收率为99.9%~104%,测定值的相对标准偏差(n=6)为1.9%~3.5%。
Abstract
The grape sample was weighed and put into the headspace bottle with sodium chloride added in advance. The saturated potassium hydroxide solution was added then. GC was applied to the determination of residual amount of ethephon in the above mixture with headspace. The temperature and time of headspace were set at 75℃ and 90 min. The analyte was separated on HP-5 chromatographic column (30 m×0.32 mm, 0.25 μm) and detected by hydrogen flame ionization detector. Linear relationship between values of peak area and mass concentration of ethephon was kept in the range of 0.500-50.0 mg·L-1, with detection limit (3S/N) of 0.010 0 mg·kg-1. The proposed method was applied to the analysis of the grape sample, giving values of recovery found by standard addition method and RSDs (n=6) of determined values in the ranges of 99.9%-104% and 1.9%-3.5% respectively.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202002007
所属栏目 工作简报
基金项目 工业发酵微生物重庆市重点实验室(重庆科技学院)开放基金(2018-21);重庆科技学院生活垃圾资源化处理协同创新中心项目(SHLJZYH 2018-005)
收稿日期 2019/7/2
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备注冉琴,硕士研究生,研究方向为环境检测
引用该论文: RAN Qin,LIU Jie,YANG Xiaofeng,LEI Shaorong,CHENG Zhu,DENG Xing,SU Xiaodong. GC Determination of Residual Amount of Ethephon in Grapes with Headspace[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(2): 161~164
冉琴,刘洁,杨晓凤,雷绍荣,成祝,邓星,苏小东. 顶空-气相色谱法测定葡萄中乙烯利的残留量[J]. 理化检验-化学分册, 2020, 56(2): 161~164
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参考文献
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【3】张莹,丁春瑞,鹿毅.HPLC-MS/MS法测定果蔬中乙烯利的残留[J].新疆农业科学, 2015,52(1):157-161.
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【5】GUO Z X, CAI Q T, YANG Z G. Ion chromatography/inductively coupled plasma mass spectrometry for simultaneous determination of glyphosate,glufosinate, fosamine and ethephon at nanogram levels in water[J]. Rapid Communications in Mass Spectrometry, 2007,21(10):1606-1612.
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