Citation: TANG Shengyun, WANG Yuanxing, WEN Pingwei, XIN Zhen. Determination of N-carbamyl-L-glutamic acid in feedstuff by high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2014, 32(2): 184-188. doi: 10.3724/SP.J.1123.2013.09027 shu

Determination of N-carbamyl-L-glutamic acid in feedstuff by high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry

1.
State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047, China

Corresponding author: WANG Yuanxing,
Received Date: 18 September 2013
Available Online: 19 November 2013
Fund Project: 南昌大学食品科学与技术国家重点实验室自由探索课题(SKLF-TS-200915). (SKLF-TS-200915)

A method was developed for the determination of N-carbamyl-L-glutamic acid (NCG) in feedstuff by high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). The feedstuff samples were extracted with methanol, cleaned-up by a ProElut mixed-mode of strong anion exchange inverse column (PXA). Then the samples were separated with HPLC and detected with MS/MS in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI⁺). The fragment ions of m/z 148.0 and m/z 84.0 were used for qualitative analysis, and m/z 130.0 was selected for quantitative analysis. The limit of detection for NCG was 24 μg/kg (S/N >3), and the limit of quantification was 80 μg/kg (S/N >10). The standard calibration curve was linear over the range of 20-1000 μg/L, and the correlation coefficient was 0.9999. The recoveries of NCG in feedstuff were 104.0%, 103.5%, 95.3%, at the three spiked levels of 80, 200, 500 mg/kg with the relative standard deviations (RSDs) of 7.5%, 6.3% and 5.8%. The results showed that the method is simple, fast, highly sensitive, specific and with good purification effect. It can be applied to the analysis and determination of NCG in feedstuff.
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