Enantioselective Determination of Protein Amino Acids in Fertilizers by Liquid Chromatography鈥揟andem Mass Spectrometry on Chiral Teicoplanin Stationary Phase
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- 作者：Lukas Taujenis ; Vilma Ol拧auskait臈 ; Audrius Padarauskas
- 刊名：Journal of Agricultural and Food Chemistry
- 出版年：2014
- 出版时间：November 19, 2014
- 年：2014
- 卷：62
- 期：46
- 页码：11099-11108
- 全文大小：419K
- ISSN：1520-5118
文摘
High-performance liquid chromatography on a glycopeptide antibiotic teicoplanin-based chiral stationary phase coupled with tandem mass spectrometry was developed for fast and reliable enantioseparation and determination of protein amino acids in hydrolyzed fertilizer samples. The effect of the mobile phase parameters (type and content of organic modifier and pH) and the column temperature on the enantioselectivity was investigated. Under optimized conditions, the majority (15 of 19) of d/l-amino acid pairs were resolved with a resolution factor (Rs) higher than 1.5 with a run time of 15 min. A triple quadrupole tandem mass spectrometer operating in multiple reaction monitoring mode with an electrospray ionization (ESI) ion source was employed for detection. The method was validated in terms of linearity, limits of detection, limits of quantitation, precision, and accuracy. Linear responses were obtained with determination coefficients higher than 0.998 for all analytes, and limits of detection were from 0.04 to 0.24 渭g/mL. Sample spike/recovery experiments gave recovery values ranging from 73% for d-threonine to 116% for l-tryptophan. Relative standard deviations for inter- and intraday precision experiments were lower than 21.7%. The developed method was successfully applied for determination of the free amino acid enantiomers in five commercially available hydrolyzed protein fertilizer samples.