色谱 ›› 2021, Vol. 39 ›› Issue (12): 1340-1346.DOI: 10.3724/SP.J.1123.2021.01032

• 研究论文 • 上一篇    下一篇

气相色谱法测定中华绒螯蟹中脂肪酸组成与含量

申兆栋1,2, 黄冬梅2,*(), 方长玲2, 叶洪丽2, 田良良2, 伍姿1,2, 张俊1,2   

  1. 1.上海海洋大学食品学院, 上海 201306
    2.中国水产科学研究院东海水产研究所, 农业部远洋与极地渔业创新重点实验室, 上海 200090
  • 收稿日期:2021-01-29 出版日期:2021-12-08 发布日期:2021-06-08
  • 通讯作者: 黄冬梅
  • 作者简介:*E-mail: hdm2001@126.com.
  • 基金资助:
    2020年农业国家标准和行业标准制修订项目(农质标函[2020]128号);中央级公益性科研院所基本科研业务费资助项目(中国水产科学研究院)(2020TD72)

Determination of fatty acids compositions and contents in Chinese mitten crabs by gas chromatography

SHEN Zhaodong1,2, HUANG Dongmei2,*(), FANG Changling2, YE Hongli2, TIAN Liangliang2, WU Zi1,2, ZHANG Jun1,2   

  1. 1. College of Food Sciences and Technology, Shanghai Ocean University, Shanghai 201306, China
    2. Key Laboratory of Ocean and Polar Fisheries Innovation, Ministry of Agriculture, East China Sea Fishery Research Institute, Chinese Academy of Fishery Sciences, Shanghai 200090, China
  • Received:2021-01-29 Online:2021-12-08 Published:2021-06-08
  • Contact: HUANG Dongmei
  • Supported by:
    2020 Agricultural National Standards and Industry Standards Development and Revision Project(Agricultural Quality Standard Letter [2020] No. 128);Central Public-Interest Scientific Institution Basal Research Funded Projects (Chinese Academy of Fishery Sciences)(2020TD72)

摘要:

中华绒螯蟹中脂肪酸组成与含量的测定对评估其营养价值与品质具有重要意义,但面对种类繁多的脂肪酸提取试剂和甲酯化试剂,测定结果参差不齐,很难对中华绒螯蟹中丰富的脂肪酸准确定量。研究通过比较4种常见的脂肪提取试剂、2种脂肪酸甲酯化试剂,确定以氯仿-甲醇(1∶1, v/v)为提取试剂,含2%硫酸的甲醇溶液为甲酯化试剂,建立了测定中华绒螯蟹肌肉中脂肪酸组成与含量的气相色谱分析方法。实验按照程序升温的条件,采用DM-2560毛细管色谱柱(100 m×0.25 mm×0.20 μm)分离37种脂肪酸,氢火焰离子化检测器(FID)检测,外标法定量。37种脂肪酸在0.5~100.0 μg/mL范围内线性关系良好,其相关系数(R2)为0.9981~0.9999,检出限(LOD)与定量限(LOQ)分别为0.01~0.02 mg/100 g和0.04~0.06 mg/100 g;以棕榈酸和硬脂酸进行加标回收验证,在1、2、10 mg/100 g 3个加标水平下的加标回收率为76.0%~97.5%,相对标准偏差(RSD, n=5)为3.31%~7.90%。该方法应用于中华绒螯蟹肌肉中脂肪酸组成与含量的测定,肌肉中共测得31种脂肪酸,碳链长度为12~24,脂肪酸总含量为281.03 mg/100 g,其中油酸、二十二碳六烯酸、二十碳五烯酸等为中华绒螯蟹肌肉中主要脂肪酸。该方法操作简便,试剂、样品用量少,且定性可靠,定量准确,能检测较多的脂肪酸种类,适用于中华绒螯蟹肌肉中脂肪酸组成与含量的快速检测。

关键词: 气相色谱法, 脂肪酸, 中华绒螯蟹

Abstract:

Determination of fatty acid compositions and contents in Chinese mitten crabs is of great significance to evaluate its nutritional value and quality. However, in the face of a wide range of fatty acid extraction and methyl esterification reagents, the measurement results are uneven, and it is difficult to accurately quantify the rich fatty acids in Chinese mitten crabs. In this paper, four kinds of oil extraction reagents and two kinds of methylating reagents, were investigated. Chloroform-methanol (1∶1, v/v) was used as the extraction solvent, and methanol containing 2% sulfuric acid was used as the derivatization reagent. A method for the determination of fatty acids in the muscle of Chinese mitten crabs by gas chromatography was established. The experiment was carried out under the condition of programmed temperature rise, 37 kinds of fatty acids were separated on a DM-2560 capillary column (100 m×0.25 mm×0.20 μm), detected by hydrogen flame ionization detector (FID) and quantified by external standard method. The linear relationships of the 37 fatty acids were good in the range of 0.5-100.0 μg/mL. The correlation coefficients (R2) were 0.9981-0.9999. The limits of detection (LODs) and limits of quantification (LOQs) were 0.01-0.02 mg/100 g and 0.04-0.06 mg/100 g, respectively. The methodology was validated by palmitic acid and stearic acid. The recoveries were 76.0%-97.5%, and the relative standard deviations (RSD, n=5) were 3.31%-7.90% at the spiked levels of 1, 2 and 10 mg/100 g. The method was applied to the determination of fatty acid compositions and contents in the muscle of Chinese mitten crabs. A total of 31 kinds of fatty acids were detected. The length of carbon chain ranged from 12 to 24, and the total content of fatty acids reached 281.03 mg/100 g. Oleic acid, docosahexaenoic acid and eicosapentaenoic acid were the main fatty acids in the muscle of Chinese mitten crabs. Thus, this method provided accurate and reliable theoretical data for the determination of fatty acids in Chinese mitten crabs. This method has the advantages of simple operation, small amount of reagent and sample, reliable qualitative, accurate quantitative, detection of more fatty acid types. It is suitable for the rapid detection of fatty acid compositions and contents in muscle tissue of Chinese mitten crabs.

Key words: gas chromatography (GC), fatty acids, Chinese mitten crabs

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