色谱

色谱 ›› 2016, Vol. 34 ›› Issue (5): 520-527.DOI: 10.3724/SP.J.1123.2016.01003

• 研究论文 • 上一篇    下一篇

气相色谱-质谱联用法检测母乳脂肪中反式脂肪酸

林麒1, 李国波2, 葛品2, 许榕仙3, 林国斌1   

  1. 1. 福建省人兽共患病研究重点实验室(福建省疾病预防控制中心), 福建 福州 350001;
    2. 福建省妇幼保健院(福建省妇儿医院), 福建 福州 350001;
    3. 福建医科大学公共卫生学院, 福建 福州 350108
  • 收稿日期:2016-01-03 出版日期:2016-05-08 发布日期:2012-12-18
  • 通讯作者: 林国斌
  • 基金资助:

    福建省科技重大专项(2013YZ0002-1);福建省医药创新课题项目(2014-CXB-7).

Determination of trans-fatty acid isomers in human milk fat by gas chromatography-mass spectrometry

LIN Qi1, LI Guobo2, GE Pin2, XU Rongxian3, LIN Guobin1   

  1. 1. Fujian Provincial Key Laboratory of Zoonosis Research(Fujian Center for Disease Control & Prevention), Fuzhou 350001, China;
    2. Fujian Maternal and Child Health Care Hospital(Fujian Women and Children's Hospital), Fuzhou 350001, China;
    3. Public Health School of Fujian Medical University, Fuzhou 350108, China
  • Received:2016-01-03 Online:2016-05-08 Published:2012-12-18
  • Supported by:

    Science and Technology Important Project in Fujian Province (No. 2013YZ0002-1); Pharmaceutical Innovation Subject in Fujian Province (No. 2014-CXB-7).

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112

被引次数

6

摘要：

建立了母乳中反式脂肪酸(TFAs)的气相色谱-质谱(GC-MS)检测方法,并应用于母乳脂肪中TFAs的检测。母乳用氨水水解,乙醚和石油醚提取脂肪,提取的脂肪加入C21: 0内标,用三氟化硼甲醇溶液在80℃水浴中冷凝回流15 min进行甲酯化,正己烷提取,上清液用GC-MS分析,内标法定量。在低、中、高加标水平上验证方法的准确度与精密度,结果显示该方法可用于母乳中18种TFAs及其同分异构体的检测,其中12种TFAs在母乳脂肪中的方法检出限为4.0~47.1 mg/kg,回收率为80%~113%, RSD为2.9%~14.5%(n=6)。TFAs在部分母乳脂样品中检出,含量为9.54~6.9 mg/kg。该方法定性、定量准确,可有效用于母乳中TFAs的检测,但仍存在脂肪酸本底干扰等问题,可结合银离子固相萃取柱预分离技术进一步完善。

关键词: 反式脂肪酸, 母乳, 气相色谱-质谱, 脂肪

Abstract:

A method for the determination of trans-fatty acid isomers in human milk fat was developed by gas chromatography-mass spectrometry (GC-MS), and applied to analyze TFAs in human milk fat. The fat was extracted with diethylether and petroleum ether after ammonia hydrolysis of human milk. C21: 0 internal standard and boron trifluoride methanol solution were added to the extract for fat esterification. The solution then was refluxed in 80℃ water bath for 15 min. Finally the trans-fatty acid methyl ester isomers were extracted with hexane, and analyzed by GC-MS. GC conditions were as follows: an HP-88 column (100 m×0.25 mm×0.2 μ m) with inlet temperature of 260℃, at a split ratio of 10: 1, and a He flow rate of 1 mL/min. The initial column temperature was 140℃ (held for 5 min), then raised up to 240℃ at a rate of 4℃/min (held for 15 min). The electronic ionization (EI) source energy was 70 eV, with auxiliary (AUX) temperature of 280℃, ion source temperature of 230℃, quadrupole temperature of 150℃ in selected ion monitoring (SIM) mode. This method can analyze the 18 TFAs. The method detection limits (MDLs) of 12 TFAs were 4.0-47.1 mg/kg, and the average recoveries were 80%-113% with the relative standard deviation (RSD, n=6) range of 2.9%-14.5%. TFAs were detected in some real samples and the contents were 9.5-46.9 mg/kg. The method is reliable and sensitive, and would be better if the background interference of fatty acids should be diminished by silver ion solid phase extraction.

Key words: trans-fatty acids (TFAs), fat, gas chromatography-mass spectrometry (GC-MS), human milk

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