色谱

色谱 ›› 2010, Vol. 28 ›› Issue (08): 782-785.DOI: 10.3724/SP.J.1123.2010.00782

• 研究论文 • 上一篇    下一篇

气相色谱-质谱技术分析香稻特征化合物2-乙酰基吡咯啉

应兴华1*, 徐霞1, 陈铭学1, 欧阳由男2*, 朱智伟1, 闵捷1   

  1. 1. 中国水稻研究所农业部稻米及制品质量监督检验测试中心, 浙江 杭州 310006; 2. 中国水稻研究所稻作技术研究与发展中心, 浙江 杭州 310006
  • 收稿日期:2010-04-02 修回日期:2010-05-26 出版日期:2010-08-28 发布日期:2010-08-28
  • 通讯作者: 应兴华,助理研究员,研究方向为农产品质量安全及有机化合物解析.欧阳由男,副研究员,研究方向为稻种资源创新.
  • 基金资助:

    国家自然科学基金项目(No. 30700486)和浙江省分析测试科技计划项目(No. 2008F70016).

Determination of 2-acetyl-1-pyrroline in aroma rice using gas chromatography-mass spectrometry

YING Xinghua1*, XU Xia1, CHEN Mingxue1, OUYANG Younan2*, ZHU Zhiwei1, MIN Jie1   

  1. 1. Rice Product Quality Supervision and Inspection Center, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China; 2. Center for Rice Technology Research and Development, China National Rice Research Institute, Hangzhou 310006, China
  • Received:2010-04-02 Revised:2010-05-26 Online:2010-08-28 Published:2010-08-28

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656

被引次数

32

摘要： 建立了气相色谱-质谱技术(GC-MS)分析香稻特征化合物2-乙酰基吡咯啉的方法。在香稻中加入内标物2,4,6-三甲基吡啶,密闭,经无水乙醇-二氯甲烷(体积比为1:1)在80 ℃水浴中提取3 h。考察了温度和时间对2-乙酰基吡咯啉提取的影响。提取液经毛细管气相色谱柱HP-5MS(30 m×0.25 mm×0.25 μm)分离,全扫描监测模式GC-MS测定。以内标物计,方法的平均回收率为82.57%,相对标准偏差为5.09%,最低检出限为0.01 mg/kg。将该方法应用于11份香稻育种材料中2-乙酰基吡咯啉的测定,结果表明,清香米、泰香R207、Texmati、桂香丝糯和中健2号等5个品种中含有2-乙酰基吡咯啉,含量分别为0.097、0.098、0.699、0.045和0.047 mg/kg。该方法样品处理简单、快速、灵敏、样本和试剂消耗少,尤其适合于通过测定2-乙酰基吡咯啉含量进行香稻育种前的大批量品种筛选。

关键词: 2-乙酰基吡咯啉, 气相色谱-质谱法, 香稻

Abstract: A gas chromatography-mass spectrometry method was developed for the determination of 2-acetyl-1-pyrroline in aroma rice. 2,4,6-Trimethylpyridine （TMP） was added into the sample of aroma rice as internal standard, and the compound was extracted by the mixture of anhydrous ethyl alcohol and methylene chloride (1:1, v/v) at 80 ℃ for 3 h under sealed condition in water bath. The effects of the temperature and time on the extraction were investigated. The analyte was separated and determined using gas chromatography-mass spectrometry on an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) in scan monitoring mode. Calculated as 2,4,6-trimethylpyridine, the average recovery of the method was 82.57% with the relative standard deviation of 5.09%, and the detection limit of method was 0.01 mg/kg. The method was employed for the determination of 2-acetyl-1-pyrroline in 11 aroma rice breeding varieties. The results showed that 2-acetyl-1-pyrroline was detected in 5 aroma rice varieties, including Qingxiangmi, Taixiang R207, Texmati, Guixiangsinuo and Zhongjian 2, with the contents of 0.097, 0.098, 0.699, 0.045 and 0.047 mg/kg, respectively. The method is simple, rapid and sensitive with low sample and reagent consumption. It is suitable for screening a lot of aroma rice varieties in breeding through the determination of 2-acetyl-1-pyrroline content.

Key words: 2-acetyl-1-pyrroline, aroma rice, gas chromatography-mass spectrometry (GC-MS)