时秋娜,刘占芳,朱军.全二维气相色谱-质谱法检测动植物油[J].中国油脂,2017,42(6):.[SHI Qiuna1,LIU Zhanfang,ZHU Jun.Detection of fatty acids in animal fats and vegetable oils by comprehensive two-dimensional gas chromatography coupled with mass spectrometry[J].China Oils and Fats,2017,42(6):.]
全二维气相色谱-质谱法检测动植物油
Detection of fatty acids in animal fats and vegetable oils by comprehensive two-dimensional gas chromatography coupled with mass spectrometry
  
DOI:
中文关键词:  全二维气相色谱-质谱联用法  动植物油  脂肪酸组成
英文关键词:comprehensive two-dimensional gas chromatography coupled with mass spectrometry  animal fat and vegetable oil  fatty acid composition
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时秋娜,刘占芳,朱军  
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中文摘要:
      为建立动植物油的全二维气相色谱-质谱分析方法,选用四甲基氢氧化铵(25%)的无水甲醇(体积比1∶?50)对样品进行甲酯化衍生,对二维色谱柱、程序升温、质量扫描范围、冷吹流量、调制周期进行优化。结果表明:在调制周期5 s,冷吹流量3 L/min,DB-5MS(30 m×0.25 mm×0.25 μm)为一维柱,BP20(2.5 m×0.1 mm×0.1 μm)为二维柱,质量扫描范围(m/z)71~385,程序升温为初始温度40?℃,保持2 min,以30?℃/min升温至190?℃,再以2?℃/min升温至280?℃,保持15 min的条件下,动植物油中的脂肪酸组成得到了有效分离和准确检测,比气相色谱-质谱法灵敏度、分离效果均提高。为动植物油的进一步鉴别提供新的分析方法。
英文摘要:
      The fatty acids in animal fats and vegetable oils could be effectively detected by comprehensive two-dimensional gas chromatography coupled with mass spectrometry(GC×GC-MS). After methylation of fatty acids with methanol solution of TMAH (volumn ratio 1∶?50), the second column, temperature programming, mass scanning range, cold blow flow and modulation period were optimized. The results showed that under the conditions of column set of DB-5MS(30 m×0.25 mm×0.25 μm)as the first column, BP20(2.5 m×0.1 mm×0.1 μm)as the second column, modulation period 5 s, cold blow flow 3 L/min, mass scanning range (m/z) 71-385,temperature programming from 40?℃(2 min) to 190?℃ at 30?℃/min, from 190?℃ to 280?℃ (15 min)at 2?℃/min, the fatty acid compositions of animal fats and vegetable oils were separated effectively and determined accurately. Compared with GC-MS, GC×GC-MS method was more sensitive and had better separation effect, which could be the effective method to discriminate different animal fats and vegetable oils.
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