Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS)

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	Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS)
	Suo, Yourui; Zhao, Xianen; You, Jinmao; Wang, Honglun; Li, Yulin; Ding, Chenxu; Liu, Yongjun
	2007
发表期刊	JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
卷号	30 期号:9-12 页码:1811-1831
文章类型	Article
摘要	A sensitive method for the determination of 30 kinds of free fatty acids (FFAs, C-1-C-30) with 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4,5-f] 9,10-phenan- threne (TSPP) as labeling reagent and using high performance liquid chromatography with fluorescence detection and identification by online postcolumn mass spectrometry with atmospheric pressure chemical ionization (APCI) source in positive-ion mode (HPLC/MS/APCI) has been developed. TSPP could easily and quickly label FFAs in the presence of K2CO3 catalyst at 90 degrees C for 30 min in N,N-dimethylformamide (DMF) solvent, and maximal labeling yields close to 100% were observed with a 5-fold excess of molar reagent. Derivatives were stable enough to be efficiently analyzed by high performance liquid chromatography. TSPP was introduced into fatty acid molecules and effectively augmented MS ionization of fatty acid derivatives and led to regular MS and MS/MS information. The collision induced cleavage of protonated molecular ions formed specific fragment ions at m/z [MH](+)(molecular ion), m/z [M'+CH2CH2](+)(M' was molecular mass of the corresponding FFA) and m/z 295.0 (the, mass of protonated molecular core structure of TSPP). Fatty acid derivatives were separated on a reversed-phase Eclipse XDB-C-8 column (4.6 x 150 mm, 5 mu m, Agilent) with a good baseline resolution in combination with a gradient elution. Linear ranges of 30 FFAs are 2.441 x 10(-3) to 20 mu mol/L, detection limits are 3.24 similar to 36.97 fmol (injection volume 10 mu L, at a signal-to-noise ratio of 3, S/N 3:1). The mean interday precision ranged from 93.4 to 106.2% with the largest mean coefficients of variation (R.S.D.) < 7,5%. The mean intraday precision for all standards was < 6.4% of the expected concentration. Excellent linear responses were observed with correlation coefficients of > 0.9991. Good compositional data could be obtained from the analysis of extracted fatty acids from as little as 200 mg of bryophyte plant samples.Therefore, the facile TSPP derivatization coupled with HPLC/MS/APCI analysis allowed the development of a highly sensitive method for the quantitation of trace levels of short and long chain fatty acids from biological and natural environmental samples.; A sensitive method for the determination of 30 kinds of free fatty acids (FFAs, C-1-C-30) with 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4,5-f] 9,10-phenan- threne (TSPP) as labeling reagent and using high performance liquid chromatography with fluorescence detection and identification by online postcolumn mass spectrometry with atmospheric pressure chemical ionization (APCI) source in positive-ion mode (HPLC/MS/APCI) has been developed. TSPP could easily and quickly label FFAs in the presence of K2CO3 catalyst at 90 degrees C for 30 min in N,N-dimethylformamide (DMF) solvent, and maximal labeling yields close to 100% were observed with a 5-fold excess of molar reagent. Derivatives were stable enough to be efficiently analyzed by high performance liquid chromatography. TSPP was introduced into fatty acid molecules and effectively augmented MS ionization of fatty acid derivatives and led to regular MS and MS/MS information. The collision induced cleavage of protonated molecular ions formed specific fragment ions at m/z [MH](+)(molecular ion), m/z [M'+CH2CH2](+)(M' was molecular mass of the corresponding FFA) and m/z 295.0 (the, mass of protonated molecular core structure of TSPP). Fatty acid derivatives were separated on a reversed-phase Eclipse XDB-C-8 column (4.6 x 150 mm, 5 mu m, Agilent) with a good baseline resolution in combination with a gradient elution. Linear ranges of 30 FFAs are 2.441 x 10(-3) to 20 mu mol/L, detection limits are 3.24 similar to 36.97 fmol (injection volume 10 mu L, at a signal-to-noise ratio of 3, S/N 3:1). The mean interday precision ranged from 93.4 to 106.2% with the largest mean coefficients of variation (R.S.D.) < 7,5%. The mean intraday precision for all standards was < 6.4% of the expected concentration. Excellent linear responses were observed with correlation coefficients of > 0.9991. Good compositional data could be obtained from the analysis of extracted fatty acids from as little as 200 mg of bryophyte plant samples.
关键词	Derivatization 1-[2-(P-toluenesulfonate)-ethyl]-2-phenylimidazole-[4 High Performance Liquid Chromatography 5-f]-9 Fluorescence Detection 10-phenan- Threne (Tspp) Fatty Acids Mass Spectrometry
WOS标题词	Science & Technology ; Life Sciences & Biomedicine ; Physical Sciences
学科领域	生物化学
关键词[WOS]	PERFORMANCE LIQUID-CHROMATOGRAPHY ; CARBOXYLIC-ACIDS ; LABELING REAGENT ; TRIFLUOROMETHANESULFONATE ; IDENTIFICATION ; DERIVATIVES ; LIVERWORTS ; JAPANESE ; 9-ANTHRYLDIAZOMETHANE ; SERUM
收录类别	SCI
语种	英语
WOS研究方向	Biochemistry & Molecular Biology ; Chemistry
WOS类目	Biochemical Research Methods ; Chemistry, Analytical
WOS记录号	WOS:000246884000043
引用统计	被引频次：3[WOS] [WOS记录] [WOS相关记录]
文献类型	期刊论文
条目标识符	http://210.75.249.4/handle/363003/1273
专题	中国科学院西北高原生物研究所
作者单位	Chinese Acad Sci, NW Plateau Inst Biol, Xining 810001, Peoples R China
推荐引用方式 GB/T 7714	Suo, Yourui,Zhao, Xianen,You, Jinmao,et al. Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS)[J]. JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,2007,30(9-12):1811-1831.
APA	Suo, Yourui.,Zhao, Xianen.,You, Jinmao.,Wang, Honglun.,Li, Yulin.,...&Liu, Yongjun.(2007).Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS).JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES,30(9-12),1811-1831.
MLA	Suo, Yourui,et al."Determination of free fatty acids in soil and bryophyte plants by precolumn derivatization via HPLC with fluorescence detection and tandem mass spectrometry (HPLC-MS/MS)".JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES 30.9-12(2007):1811-1831.

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