食品科学 ›› 2018, Vol. 39 ›› Issue (8): 155-159.doi: 10.7506/spkx1002-6630-201808025

• 成分分析 • 上一篇    下一篇

高效液相色谱-电感耦合等离子质谱法分析富硒茶叶中硒的形态

陈贵宇,潘煜辰,李清清,冷桃花*,李君绩,葛宇   

  1. (上海市质量监督检验技术研究院,国家食品质量监督检验中心(上海),上海 200233)
  • 出版日期:2018-04-25 发布日期:2018-04-17
  • 基金资助:
    上海市科学技术委员会研发平台专项(上海市食品质量安全检测与评价专业技术服务平台)(15DZ2292500)

Speciation Analysis of Selenium in Selenium-Enriched?Tea by HPLC-ICP-MS

CHEN Guiyu, PAN Yuchen, LI Qingqing, LENG Taohua*, LI Junji, GE Yu   

  1. (National Food Quality Supervision and Inspection Center (Shanghai), Shanghai Institute of Quality Inspection and Technical Research, Shanghai 200233, China)
  • Online:2018-04-25 Published:2018-04-17

摘要: 建立富硒茶叶中硒代胱氨酸(SeCys2)、甲基-硒代半胱氨酸(SeMC)、亚硒酸根(Se(IV))、硒代蛋氨酸(SeMet)、硒酸根(Se(VI))5?种硒化合物的高效液相色谱-电感耦合等离子体质谱的分离检测方法。方法利用Hamilton?PRP-X100色谱柱对富硒茶叶中5?种硒化合物进行分离,利用电感耦合等离子体质谱对硒元素进行检测,外标法定量测定5?种硒化合物的含量。研究采用蛋白酶K溶液为提取剂,超声提取60?min,以柠檬酸溶液为流动相,梯度洗脱,5?种硒化合物在15?min内得到了有效分离。5?种硒化合物标准曲线的线性相关系数不小于0.999?8,检出限为0.13~1.09?μg/L。该前处理方法样品加标回收率在91.8%~109.4%之间。方法操作简便、分离效果好、检出限低,适用于富硒茶叶中硒的形态分析。

关键词: 高效液相色谱-电感耦合等离子质谱, 硒, 形态分析, 富硒茶叶

Abstract: A method for the determination of 5 selenium species (SeCys2, SeMC, Se(IV), SeMet, and Se(VI)) in selenium-enriched tea was established using high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). A Hamilton PRP-X100 column was used to separate the five compounds using citric acid as the mobile phase. Quantification was performed by the external standard method. The five selenium compounds were ultrasonically extracted using 1 mL of protease K (10 mg/mL) for 60 minutes, and then separated with gradient?elution in 15 min. The correlation coefficients of the standard curves were larger than 0.999 8, and the limits of detection (LODs) were in the range of 0.13–1.09 μg/L. The spiked recoveries ranged from 91.8% to 109.4%. The method allowed simultaneous determination of selenium compounds in selenium-enriched?tea with simple and convenient operation, efficient separation and low detection limit.

Key words: high performance liquid chromatography-inductively coupled plasma-mass spectrometry, selenium, speciation analysis, selenium-enriched?tea

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