GC-MS同时测定不同产地羊脂油中10种脂肪酸类成分
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摘要
目的:测定中药炮制辅料-羊脂油中主要的脂肪酸类成分含量,比较不同产地羊脂油的脂肪酸成分含量,为其质量控制提供重要技术支撑。方法:样品经柱前衍生化后采用GC-MS联用技术,DB-5 MS非极性色谱柱(30 m×0. 25 mm×0. 25μm),程序升温,选择离子扫描模式(SIM)同时测定羊脂油中10种脂肪酸成分。结果:10种脂肪酸中十二烷酸甲酯(DODME)浓度在0. 010～10. 0μg·ml~(-1),十四烷酸甲酯(MTEME)浓度在0. 013～12. 8μg·ml~(-1),十五烷酸甲酯(PENME)浓度在0. 011～12. 0μg·ml~(-1),9-十六碳烯酸甲酯(9-HEXME)浓度在0. 020～20. 0μg·ml~(-1),棕榈酸甲酯(HEXME)浓度在0. 048～50. 0μg·ml~(-1),十七烷酸甲酯(HEPME)浓度在0. 013～13. 0μg·ml~(-1),9,12-十八碳二烯酸甲酯(9,12-OCME)浓度在0. 020～20. 0μg·ml~(-1),9-十八碳烯酸甲酯(9-OCME)浓度在0. 020～20. 0μg·ml~(-1),硬脂酸甲酯(OCTME)浓度在0. 030～32. 0μg·ml~(-1),二十烷酸甲酯(EICME)浓度在0. 010～10. 8μg·ml~(-1)均具有很好的线性(r≥0. 999 9),定量限(LOQ)为1. 25～5. 95μg·L-1,回收率在82. 1%～98. 7%;通过测定18批羊脂油中的10种主要脂肪酸成分,测定结果表明,含量最高的为棕榈酸(3. 79%～13. 22%),硬脂酸(3. 41%～18. 11%)和油酸(4. 48%～6. 28%,部分批次样品中未检测到)。结论:该方法稳定、可靠、重复性好,可用于羊脂油的含量测定和质量控制。
Objective: To determine the contents of major fatty acid components in sheep fat( SF),and compare the fatty acid contents of sheep fat from different producing areas to provide important technical support for the quality control. Methods: The samples were pre-column derivatized and determined by GC-MS with a DB-5 MS non-polar column(30 m × 0. 25 mm,0. 25 μm),temperature-programmed program and SIM mode,and 10 kinds of fatty acid were simultaneously detected. Results: DODME(0. 010 ～ 10. 0 μg·ml~(-1)),MTEME(0. 013 ～ 12. 8 μg·ml~(-1)),PENME(0. 011 ～ 12. 0 μg·ml~(-1)),9-HEXME(0. 020 ～ 20. 0μg·ml~(-1)),HEXME(0. 048 ～ 50. 0 μg·ml~(-1)),HEPME(0. 013 ～ 13. 0 μg·ml~(-1)),9,12-OCME(0. 020 ～ 20. 0 μg·ml~(-1)),9-OCME(0. 020 ～ 20. 0 μg·ml~(-1)),OCTME(0. 030 ～ 32. 0 μg·ml~(-1)) and EICME(0. 010 ～ 10. 8 μg·ml~(-1)) had a good linear relationship within the corresponding concentration range( r ≥ 0. 999 9). The quantitative limit( LOQ) was 1. 25-5. 95 μg·L-1,and the recovery was 82. 1%-98. 7%. The determination of 10 major fatty acid components in 18 batches of sheep fat showed that palmitic acid(3. 79%-13. 22%),stearic acid(3. 41%-18. 11%) and oleic acid(4. 4 8%-6. 28%,not detected out in some batch samples) were with the highest contents. Conclusion: The method is stable,reliable and reproducible. It can be used for the determination and quality control of sheep fat oil.
Objective: To determine the contents of major fatty acid components in sheep fat( SF),and compare the fatty acid contents of sheep fat from different producing areas to provide important technical support for the quality control. Methods: The samples were pre-column derivatized and determined by GC-MS with a DB-5 MS non-polar column(30 m × 0. 25 mm,0. 25 μm),temperature-programmed program and SIM mode,and 10 kinds of fatty acid were simultaneously detected. Results: DODME(0. 010 ～ 10. 0 μg·ml~(-1)),MTEME(0. 013 ～ 12. 8 μg·ml~(-1)),PENME(0. 011 ～ 12. 0 μg·ml~(-1)),9-HEXME(0. 020 ～ 20. 0μg·ml~(-1)),HEXME(0. 048 ～ 50. 0 μg·ml~(-1)),HEPME(0. 013 ～ 13. 0 μg·ml~(-1)),9,12-OCME(0. 020 ～ 20. 0 μg·ml~(-1)),9-OCME(0. 020 ～ 20. 0 μg·ml~(-1)),OCTME(0. 030 ～ 32. 0 μg·ml~(-1)) and EICME(0. 010 ～ 10. 8 μg·ml~(-1)) had a good linear relationship within the corresponding concentration range( r ≥ 0. 999 9). The quantitative limit( LOQ) was 1. 25-5. 95 μg·L-1,and the recovery was 82. 1%-98. 7%. The determination of 10 major fatty acid components in 18 batches of sheep fat showed that palmitic acid(3. 79%-13. 22%),stearic acid(3. 41%-18. 11%) and oleic acid(4. 4 8%-6. 28%,not detected out in some batch samples) were with the highest contents. Conclusion: The method is stable,reliable and reproducible. It can be used for the determination and quality control of sheep fat oil.
引文
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2徐凤娟,孙娥,张振海,等.中药炮制辅料羊脂油的研究思路探析[J].中华中医药杂志,2014(8):2543-2547
3黄兰岚,李娆娆,原思通,等.中药炮制辅料羊脂油质量标准研究进展[C].河南焦作:中华中医药学会四大怀药与地道药材研究论坛暨中药炮制分会会员代表大会,2007
4 Jiang J,Jia X.Profiling of fatty acids composition in suet oil based on GC-EI-qMS and chemometrics analysis[J].Int J Mol Sci,2015,16(2):2864-2878
5 Ansorena D,Raes K,De Smet,et al.Analysis of fatty acid isomers in ruminant tissues by silver thin layer chromatography followed by gas chromatography[J].Meded Rijksuniv Gent Fak Landbouwkd Toegep Biol Wet,2001,66(3b):365-372
6 Wang A,Li G,You J,et al.A new fluorescent derivatization reagent and its application to free fatty acid analysis in pomegranate samples using HPLC with fluorescence detection[J].J Sep Sci,2014,36(24):3853-3859
7 Li A,Ha Y,Wang F,et al.Determination of thermally induced trans-fatty acids in soybean oil by attenuated total reflectance fourier transform infrared spectroscopy and gas chromatography analysis[J].J Agr Food Chem,2012,60(42):10709-10713
8 Zhang S,Sun Y,Sun Z,et al.Determination of triterpenic acids in fruits by a novel high performance liquid chromatography method with high sensitivity and specificity[J].Food Chem,2014,146:264-269