- P-ISSN 1225-0163
- E-ISSN 2288-8985
본 연구에서는 사료 첨가제로 이용되고 있는 유기산 7종(formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid, propionic acid)의 동시분석법 개발을 위한 연구를 실시하였다. 7종의화합물은 표준물질의 Retention time과 UV spectra를 통해 구별하였고, 분석법 검증은 직선성, 민감성, 선택성, 정확성, 정밀성을 통하여 검증하였다. 그 결과로 LOD와 LOQ의 범위가 각각 43~26,755 μg/kg, 12- 8,026 μg/kg으로 설정하였고, 평균 회수율이 79.3~95.2%로 우수하게 보였으며, intra-day, inter-day에 대한전반적인 상대 표준 편차(%RSD)는 3.2% 미만으로 나타났다. 이와 같이 검증된 자료를 통해 유기산의동시분석에 대한 직선성, 민감성, 선택성, 정확성 및 정밀성을 확인하였고, 높은 수준을 나타냄을 알 수있었다. 이를 바탕으로 유기산이 검출되는 단미사료 46 가지를 분석에 적용하여 진행하였고, 정량과 동시분석 검출을 위한 방법은 RP-HPLC/UV 검출기를 이용하여 성공적으로 개발되었다. 따라서 본 연구결과를 바탕으로 하여 사료 중의 유기산의 분석이 신속하고 정확해졌을 뿐 아니라, 다른 종류의 사료 또한이를 적용하여 효율적으로 이용할 수 있을 것으로 판단된다.
A novel and simple method for detecting seven organic acids (formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid and propionic acid) in animal feed using high performance liquid chromatography equipped with a photo-diode array detector (HPLC/PDA) was developed. The chromatographic peaks of the seven organic acids were successfully identified by comparing their retention times and UV spectra with reference standards. Method validation was performed in terms of linearity, sensitivity, selectivity, accuracy, and precision. The limits of detection (LODs) for the instrument employed in these experiments ranged from 12 to 8,026 μg/kg, and the limits of quantification (LOQs) ranged from 43 to 26,755 μg/kg. Average recoveries of the seven organic acids ranged from 79.3 to 95.2 %. Method replication resulted in intra- day and interday peak area variation of <3.2 %. The developed method was specific and reliable and is therefore suitable for the routine analysis of organic acids in animal feed.
1. D. W. Kim, J. H. Kim, S. K. Kim, G. H. Kang, H. K. Kang, S. J. Lee and S. H. Kim, J. Anim. Sci. Technol., 51, 207-216 (2009).
2. J. W. Joo, J. Y. Choi, S. C. Choi, W. T. Cho, B. J. Chae and Y. X. Yang, J. Anim. Sci. Technol., 51, 15-24 (2009).
3. K. H. Partanen and Z. Mro, Nutr. Res. Rev., 12, 117-145(1991).
4. I. H. Hwang, Feed Industry, 2, 58-65 (2004).
5. H. K. Yoon, Y. H. Kim and J. H. Han, Korean J. Vet. Serv., 32(1), 77-82 (2009).
6. X. Yin, Jianghua Li, H. D. Shin, Guocheng Pu, Long Liu and Jian Chen, Biotechnol. Adv., 33, 830-841(2015).
7. C. H. Lee, I. H. Jo, J. C. Shon and S. H. Lee, Korean J. Org. Agric., 17, 237-251 (2009).
8. Sung Su Ill, Ministry for Food, Agriculture, Forestry and Flsheries (MIFAFF), 506028-3 (2009).
9. Standard and specification for animal feeds, Ministry of Agriculture. Food and Rural Affairs (MAFRA), 2014-45 (2014.04.29).
10. Rodrigo Scherer, Ana Cecilia Poloni Rybka, Cristiano Augusto Ballus, Adriana Dillenburg Meinhart, Jose Teixeira Filho, Helena Teixeira Godoy, Food Chem., 135, 150-154 (2012).
11. Hans A. Eyeghe-Bickong, Erik O. Alexandersson1, Liezel M. Gouws, Philip R. Young and Melane A. Vivier, J. Chromatogr. B, 885-886, 43-49 (2012).
12. Giuseppe Zeppa, Lorenza Conterno and Vincenzo Gerbi, Agric. Food Chem., 59, 2722-2726 (2001).
13. Jorge Bouzas, Carlos A. Kantt, Floud Bodyfelt and J. Antonio, Torres, Food Sci., 56, 276-278 (1991).
14. Fabio Chinnici, Umberto Spinabelli, Claudio Riponi and Aureliano Amati, J. Feed Compos. Anal., 18, 121-130 (2005).
15. X.-Q. Wang, F.-Y. Wei, Z.-F. Wei, L. Zhang, M. Luo, Y.-H. Zhang, Y.-G. Zu and Y.-J. Fu, Sep. Purif. Technol., 35, 80-87 (2014).
16. Ute Roessner, Cornelia Wagner, Joachim Kopka, Richard N. Trethewey and Lothar Willmitzer, Plant J., 23, 131-142 (2000).
17. M.-H. Yanga and Y.-M. Choongb, Food Chem., 75, 101-108 (2001).
18. ICH International Conference Harmonization, Validation of analytical procedures: test and methodology (2005).
19. M. Thompson, S. L. R. Ellison and R. Wood, Int. Union Pure Appl. Chem.(IUPAC), 74, 835-855 (2002).