食品科学 ›› 2022, Vol. 43 ›› Issue (12): 290-294.doi: 10.7506/spkx1002-6630-20210421-302

• 安全检测 • 上一篇    

樱桃中溴形态分析方法及其在熏蒸过程追溯中的应用

吴池莹,张润何,邓晓军,盛永刚,蔡文瑄,谢敏,陈仲兵,杨晓君,赵超敏,樊祥   

  1. (上海海关,上海 200135)
  • 发布日期:2022-07-01
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1603603);上海市委科研项目(20392001700); 上海海关科研项目(SHK006-2020)

A Method for Speciation Analysis of Bromine in Cherries and Its Application for Traceability Analysis of Methyl Bromide Fumigation

WU Chiying, ZHANG Runhe, DENG Xiaojun, SHENG Yonggang, CAI Wenxuan, XIE Min, CHEN Zhongbing, YANG Xiaojun, ZHAO Chaomin, FAN Xiang   

  1. (Shanghai Customs, Shanghai 200135, China)
  • Published:2022-07-01

摘要: 建立樱桃中溴形态的分析方法,对比未熏蒸与熏蒸后樱桃中溴甲烷残留量和无机溴含量,研究溴甲烷熏蒸与溴残留的关系。采用水超声提取,以36 mmol/L硝酸+67 mmol/L氨水作为流动相,经阴离子色谱柱分离,高效液相色谱-电感耦合等离子体质谱法分析樱桃中的溴形态,并使用电感耦合等离子体质谱法确证樱桃中总溴含量,顶空进样-气相色谱法检测樱桃中溴甲烷残留量。研究表明,溴形态分析方法中溴酸根的回收率在89.7%~101.4%之间,相对标准偏差为2.1%~3.5%,溴离子回收率为85.5%~107.3%,相对标准偏差为4.4%~7.0%,定量限为0.10 mg/kg。溴甲烷熏蒸后樱桃中只含有溴离子,其含量与总溴含量相符。熏蒸后樱桃中的溴甲烷残留量随时间递减,溴离子含量明显高于未熏蒸,且不受时间与保存条件的影响产生显著变化。本方法可对樱桃的溴甲烷熏蒸过程进行追溯,为水果的进出口风险监控和质量控制提供依据。

关键词: 樱桃;溴离子;总溴;溴甲烷;熏蒸;追溯

Abstract: An analytical method for the speciation of bromine in cherries fumigated with methyl bromide was established and applied to compare the contents of methyl bromide and inorganic bromine in un-fumigated and fumigated cherries in order to explore the relationship between methyl bromide fumigation and bromine residue. The samples were ultrasonically extracted with water and the extract was separated on an anion exchange column using a mobile phase composed of 36 mmol/L nitric acid and 67 mmol/L aqueous ammonia before being analyzed by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Total bromine was determined by ICP-MS and methyl bromide by headspace sampling-gas chromatography with an electron capture detector (HS-GC-ECD). The results showed that recovery of the spiked bromate ranged from 89.7% to 101.4% with relative standard deviations (RSDs) of 2.1%?3.5%. The recoveries of the spiked bromide ion were 85.5%?107.3% with RSDs of 4.4%?7.0%. The limit of quantification of the developed method was 0.10 mg/kg. Only bromide ions were found to exist in cherries fumigated with methyl bromide and the content of bromide ions was consistent with the content of total bromine. Methyl bromide residues in fumigated cherries decreased over time. The content of total bromine in fumigated cherries was significantly higher than that in un-fumigated cherries, and did not significantly change with storage time or conditions. Therefore, this method, which is useful to trace methyl bromide fumigation of cherries, provides a basis for risk monitoring and quality control of fruit import and export.

Key words: cherry; bromide ion; total bromine; methyl bromide; fumigation; traceability

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