全二维气相色谱-质谱法检测动植物油.pdf

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CHINA OILS AND FATS
2017Vol.42No.6
检測分析
全二维气相色谱一质谱法检测动植物油
时秋娜,刘占芳,朱军,田菲菲
(1.河南警察学院刑事科学技术系,郑州450026:2.公安部物证鉴定中心,北京100038
3.岛津企业管理(中国)有限公司,北京100020)
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5s,冷吹流量3L/min,DB-5MS(30mx0.25mmx0.25um
为一维柱,BP20(2.5mx0.1mmx0.1um)为二维柱,质量扫描范围(m/z)71~38,程序升温为初始
温度40℃,保持2min,以30℃/min升温至190℃,再以2℃/min升温至280℃,保持15min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,比气相色谱一质谱法灵敏度、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。
关键词∷全二维气相色谱一质谱联用法;动植物油脂肪酸组成
中图分类号:TS225TQ646文献标识码:文章编号:1003-7969(2017)06-0138-05
Detection of fatty acids in animal fats and vegetable oils by comprehensive
two -dimensional gas chromatography coupled with mass spectrometry
SHI Qiuna', LIU Zhanfang ,ZHU Jun, TIAN Feifei
(1. Department of Criminal Science and Technology, Henan Police College, Zhengzhou 450026, China?
2. Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China
3. Shimadzu Global COE for Application & Technical Development, Beijing 100020, China)
Abstract The fatty acids in animal fats and vegetable oils could be effectively detected by comprehensive
two-dimensional gas chromatography coupled with mass spectrometry(GC x Gc-ms).After methyla
tion 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 x0.25 mm x0. 2:
um)as the first
column, BP20( 2.5 m x0. 1 mm x0. I wm)as the second column, modulation period 5 s, cold blow flow
3 L/min, mass scanning range (m/z)71-385, temperature programming from 40C(2 min)to 190
at30℃C/min,fom190℃Cto280℃(15min)at2℃/min, the fatty acid compositions of animal fats and
vegetable oils were separated effectively and determined accurately. Compared with GC-MS, GC x
GC-MS method was more sensitive and had better separation effecl, which could be the elfective method
to discriminate different animal fats and vegetable oils
Key words comprehensive two-dimensional gas chromatography coupled with mass spectrometry, ani
mal fat and vegetable oil, fatty acid composition
动植物油是人们生活中必不可少的膳食种类,和类刑事案件中常见的物证,其常以油溃斑痕、脂肪微粒
人们的日常生活联系紧密。因此,动植物油也成为各的形式遗留在案发现场,或附着在犯罪嫌疑人的衣服、
鞋子、作案工具上,对其进行分析检验,能够为案件侦
收稿日期:2016-11-03:修回日期:2017-03-23
查提供线索,为诉讼提供证据,具有十分重要的意义
作者简介:时秋娜(1979),女,讲师,硕士,研究方向为微量
目前有关动植物油脂肪酸组成的检验,常见的
物证与毒物毒品检验(-mail)752252414@qg.com。
仪器分析方法有气相色谱法、气相色谱一质谱
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