Determination of long-chain fatty acids in bryophyte plants extracts by HPLC with fluorescence detection and identification with MS

Novel Reagent for the Sensitive Determination of Free Fatty Acids by HPLC With Fluorescence Detection and Identification With Mass Spectrometry and Application to Several Medicinal Herbs

“…1-[2-(p-toluenesulfonate)ethyl]-2-phenylimi-dazole-[4,5-f]-9,10-phenanthrene (TSPP) was prepared according to the method previously described in our laboratory. [22] Synthesis of Labeling Reagent 2-(2-(4-(dimethylamino)phenyl)-1H-phenanthro[9,10-d]-imidazol-1-yl)-ethyl-4-methylbenzenesulfonate (PPMB) Synthesis of N,N-dimethyl-4-(1H-phenanthro [9,10-d]imidazol-2-yl)aniline(DPIA) N,N-Dimethyl-4-(1H-phenanthro[9,10-d]imidazol-2-yl)aniline (DPIA) was synthesized according to the method as follows: 9,10-Phenanthraquinone (10 g), 4-(dimethylamino)benzaldehyde (10 g), and ammonium acetate (74 g) were fully added in a 500-mL of round-bottom flask, which were mixed with glacial acetic acid (300 mL). The contents of the flask were heated at 80-90 C for a period of 3 hr with vigorous stirring.…”

“…[22] However, they also gave relatively low the ionization efficiency under APCI-MS in positive-ion mode as nitrogen atom in its core structure was intensively conjugated by benzene ring. This was great disadvantage to the post-column online sensitive MS identification for low contents of fatty acid compounds in real environmental samples.…”

“…The detection and identification of fatty acid derivatives were carried out by fluorescence and APCI-MS in positive-ion detection mode. Meanwhile, the fluorescence detection responses were compared with those obtained by using 1-[2-(p-toluenesulfonate)-ethyl]-2-phenylimidazole-[4,5-f]-9,10-phenanthrene (TSPP) [22] as labeling reagent previously reported in our laboratory. Linearity, detection limits, and precision of the procedure were also evaluated and compared with the reported data.…”

Recent trends in the advanced analysis of bioactive fatty acids

“…On the other hand, FL reactions can be classified into following two groups: (1) FL generation, which is generally due to the production of the FL compound from the reaction of non-FL reagent with target compound, resulting in the generation of fluorescence, and (2) FL tagging, based in the covalent binding formation between the reactive functional groups in FL reagent and target compound. A large number of FL reagents have been developed for the determination of carboxylic acids involving FFAs, among them, the bromoalkyl reagents [292]. Optimal derivatization conditions were obtained at temperatures of 90 • C for 30 min, using DMSO and K 2 CO 3 as co-solvent and basic catalyst, respectively.…”

Extraction of pollen lipids by SFE‐CO2 and determination of free fatty acids by HPLC

“…CO 2 (99.99% purity), contained in a cylinder with an eductor tube, was obtained from Fushan Co. (Yantai, China). TSPP was synthesized in our laboratory, as described previously [16].…”