| 基于离子排斥色谱的饲料酸化剂中多种有机酸同步检测 |
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| 引用本文： | 贾铮,肖志明,李兰,樊霞.基于离子排斥色谱的饲料酸化剂中多种有机酸同步检测[J].农业工程学报,2016,32(12):303-308. |
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| 作者姓名： | 贾铮 肖志明 李兰 樊霞 |
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| 作者单位： | 中国农业科学院农业质量标准与检测技术研究所,北京,100081 |
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| 基金项目： | 中国农业科学院"饲料质量安全检测与评价"创新团队项目资助。 |
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| 摘 要： | 为了规范饲用酸化剂的使用和管理,建立一种快速、准确的多种有机酸同步检测方法应需而生。该文以实现饲料酸化剂中多种有机酸的同步检测为目标,基于离子排斥色谱技术,对饲料酸化剂中多种有机酸(柠檬酸、酒石酸、苹果酸、乳酸、甲酸、乙酸、富马酸、丙酸和丁酸)的检测条件进行了优化研究。研究采用Bio-Rad Aminex HPX-87H(300mm×7.8 mmΦ,9μm)离子排斥色谱柱及二极管阵列检测器,以硫酸溶液作为流动相,比较了不同流动相浓度、不同柱温、不同流动相流速、不同检测波长等色谱条件对同步检测饲料酸化剂中9中有机酸的影响;以上述优选的条件建立分析方法,考察此方法的线性范围和检出限、回收率和精密度,并用实际样品进行了验证。研究结果表明:以0.025 mol/L硫酸溶液为流动相,流速0.70 m L/min,柱温30℃,DAD检测波长为210 nm,以保留时间结合待测物质的紫外特征吸收光谱进行定性分析,外标法进行定量分析。9种有机酸组分的质量浓度与其峰面积在一定范围内呈良好线性关系,决定系数0.999,9种有机酸组分在20 min内可以得到良好分离;方法检出限为0.01~2.4 mg/L,加标回收率为90.7%~101.1%,相对标准偏差为0.91%~3.33%。基于上述条件建立的检测方法能够满足饲料酸化剂中多种有机酸成分的同步定量分析。
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| 关 键 词： | 色谱 检测器 有机酸 二极管阵列 饲料酸化剂 同步检测 |
| 收稿时间： | 1/2/2016 12:00:00 AM |
| 修稿时间： | 2016/4/24 0:00:00 |
Simultaneous determination of multi-organic acids in feed acidifier by ion exclusion chromatography |
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| Jia Zheng,Xiao Zhiming,Li Lan and Fan Xia.Simultaneous determination of multi-organic acids in feed acidifier by ion exclusion chromatography[J].Transactions of the Chinese Society of Agricultural Engineering,2016,32(12):303-308. |
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| Authors: | Jia Zheng Xiao Zhiming Li Lan and Fan Xia |
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| Institution: | Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China,Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China,Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China and Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China |
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| Abstract: | The addition of different kinds of acidifiers into animal feed would be effective in decreasing pH value and acid-binding capacity, and thus it brings the advantages such as facilitating the digestion and absorption, and enhancing the immune function. In connection with the demands for food safety and environment-friendly production, acidifiers have received considerable attention as feed additives. Regulating the usage and management of feed acidifiers requires the establishment of a synchronous detection method for different kinds of organic acids with high speed and high accuracy. The research object of this study was to establish the synchronous detection method, and to optimize the detecting condition of 9 kinds of organic acids (citric acid, tartaric acid, malic acid, lactic acid, formic acid, acetic acid, fumaric acid, propionic acid and butyric acid) based on the ion exclusion chromatography coupled with diode array detector (DAD). All the organic acids in this study were extracted by deionized water for further detection. A Bio-Rad Aminex HPX-87H (300 mm × 7.8 mm, 9μm) ion exclusion chromatography column with DAD was applied and sulfuric acid solution was taken as the flowing phase, and the different effects of chromatographic conditions such as mobile phase, flow rate, column temperature and detecting wave length on the 9 organic acids in feed acidifiers during synchronous detection were compared and analyzed. Then, the analytical methods established for all the above mentioned parameters were investigated for their linearity range, the limit of detection, the recovery rate and precision, followed by the verification using actual samples. The results showed that the best optimized parameter conditions for synchronously detecting the 9 organic acids were 0.025 mol/L sulfuric acid solution as flowing phase, flowing speed of 0.70 mL/min, column temperature of 30℃ , and210 nm detecting wave length for DAD. The qualitative analysis of organic acids was executed based on their retention time and ultraviolet absorption spectra, while the quantitative analysis was executed based on the external standard method. According to the results of this study, it could be found that the mass concentration and the peak area had behaved nice linear correlations in specific range for the 9 organic acids, respectively, with the determination coefficients higher than 0.999. All the 9 organic acids could be successfully separated within 20 min. The limit of detection of the synchronous detection method was from 0.01 to 2.4 mg/L and the recovery rate was from 90.7% to 101.1%, while the relative standard deviation was from 0.91% to 3.33%. Bases on these results, the synchronous detection method focused in this study shows to be one of the successful ways for organic acid detecting in different animal feed acidifiers. This study can provide the technical support in further investigation of the acidifiers' application in the animal feed manufacturing factory as well as in the real market for quality assurance. |
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| Keywords: | chromatography detectors organic acids diode array detector feed acidifier simultaneous determination |
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