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中国农学通报 ›› 2025, Vol. 41 ›› Issue (34): 129-136.doi: 10.11924/j.issn.1000-6850.casb2025-0752

• 食品·营养·检测·安全 • 上一篇    下一篇

柱前衍生-高效液相色谱法测定雪茄烟叶中16种游离氨基酸的含量

周婷1,2(), 陈琦1,2, 张静3, 李萍3(), 岳小淋3, 谭文渊3, 王兰3, 晋伊乐1,2, 高云鹏1,2   

  1. 1 四川中烟工业有限责任公司长城雪茄烟厂,四川什邡 618400
    2 国产雪茄烟叶开发及工业高效利用四川省重点实验室,四川什邡 618400
    3 四川轻化工大学化学工程学院,四川自贡 643000
  • 收稿日期:2025-09-05 修回日期:2025-11-12 出版日期:2025-12-04 发布日期:2025-12-04
  • 通讯作者:
    李萍,女,1998年出生,四川广元人,在读硕士研究生,主要从事痕量分析检测研究。通信地址:64300 四川省自贡市四川轻化工大学汇南校区,E-mail:
  • 作者简介:

    周婷,女,1987年出生,四川德阳人,助理工程师,本科,主要从事雪茄烟叶工业高效利用研究。通信地址:618400 四川中烟长城雪茄烟厂技术中心,E-mail:

  • 基金资助:
    厅市共建国产雪茄烟叶工业高效利用四川省重点实验室“不同雪茄烟叶的非靶标分析”(Kf-2023-01)

Determination of 16 Free Amino Acids in Cigar Tobacco Leaves by Pre-column Derivatization-high Performance Liquid Chromatography

ZHOU Ting1,2(), CHEN Qi1,2, ZHANG Jing3, LI Ping3(), YUE Xiaolin3, TAN Wenyuan3, WANG Lan3, JIN Yile1,2, GAO Yunpeng1,2   

  1. 1 Great Wall Cigar Factory, China Tobacco Sichuan Industrial Co., Ltd., Shifang, Sichuan 618400
    2 Development & Industrial Efficient Utilization of Domestic Cigar Tobacco Key Laboratory of Sichuan Province, Shifang, Sichuan 618400
    3 School of Chemical Engineering, Sichuan University of Science and Engineering, Zigong, Sichuan 643000
  • Received:2025-09-05 Revised:2025-11-12 Published:2025-12-04 Online:2025-12-04

摘要:

游离氨基酸是雪茄烟叶中重要的风味化学成分,对其准确、快速的测定对雪茄品质评价具有重要意义。基于柱前衍生-反相高效液相色谱法,建立同时检测雪茄烟叶中16种氨基酸的方法。通过优化色谱柱温、流速、超声提取时间及衍生化时间等关键参数,明确最优检测条件;系统考察方法学性能,并应用于40份不同产区、部位、等级的雪茄烟叶样品分析,结合雷达图揭示氨基酸含量与样品属性的关联性。结果表明,16种氨基酸含量在2.5~400 mg/L范围内,线性相关系数R2≥0.998,检出限为0.014~0.096 mg/L,定量限为0.047~0.320 mg/L,加标回收率为89.05%~107.08%,相对标准偏差为1.25%~5.72%,方法准确可靠。实际样品分析显示,雪茄烟叶中氨基酸含量与产区(B地区含量整体较高)、部位(上部叶>中部叶>下部叶)、等级(二级>三级>四级)存在显著关联性。该方法操作简便、分离效果好、灵敏度高,可用于雪茄烟叶氨基酸含量检测与品质分级评价。

关键词: 柱前衍生, 高效液相色谱法, 雪茄, 氨基酸, 提取, 含量测定, 品质评价

Abstract:

Free amino acid is an important flavor chemical component in cigar leaves, and its accurate and rapid determination is of great significance for cigar quality evaluation. A method for the simultaneous determination of 16 amino acids in cigar leaves was established based on pre-column derivatization-reversed-phase high performance liquid chromatography. The optimal detection conditions were determined by optimizing the key parameters such as column temperature, flow rate, ultrasonic extraction time and derivatization time. The methodological performance was systematically investigated and applied to the analysis of 40 cigar leaf samples from different producing areas, parts and grades. The correlation between amino acid content and sample attributes was revealed by radar map. The results showed that the contents of 16 amino acids were in the range of 2.5-400 mg/L, the linear correlation coefficient R2≥0.998, the detection limit was 0.014-0.096 mg/L, the quantitative limit was 0.047-0.320 mg/L, the recovery rate was 89.05%-107.08%, and the relative standard deviation was 1.25%-5.72%. The method was accurate and reliable. The analysis of actual samples showed that the amino acid content in cigar leaves had significant correlations with the producing area (the overall content in B area was higher), the position (upper leaf> middle leaf> lower leaf), and the grade (second grade > third grade > fourth grade). The method has the advantages of simple operation, good separation effect and high sensitivity, and can be used for the detection of amino acid content and quality grading evaluation of cigar tobacco leaves.

Key words: precolumn derivatization, high performance liquid chromatography, cigar, amino acid, extraction, assaying, quality evaluation