Junsomboon Jaroon, Jakmunee Jaroon
Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200, Thailand.
Anal Chim Acta. 2008 Oct 10;627(2):232-8. doi: 10.1016/j.aca.2008.08.012. Epub 2008 Aug 23.
A simple flow injection (FI) conductometric system with gas diffusion separation was developed for the determination of Kjeldahl nitrogen (or proteins) in milk and chicken meat. The sample was digested according to the Kjeldahl standard method and the digest was diluted and directly injected into the donor stream consisting of 4M NaOH. In alkaline medium, ammonium was converted to ammonia, which diffused through the PTFE membrane to dissolve in an acceptor stream (water). Dissociation of ammonia caused a change in conductance of the acceptor solution, which was linearly proportional to the concentration of ammonium originally present in the injected solution. A conductometric flow through cell and an amplifier circuit was fabricated, which helped improve sensitivity of the conductometric detection system. With using a plumbing Teflon tape as a gas diffusion membrane and without thermostating control of the system, a linear calibration graph in range of 10-100mgL(-1) N-NH(4) was obtained, with detection limit of 1mgL(-1) and good precision (relative standard deviation of 0.3% for 11 replicate injections of 50mgL(-1) N-NH(4)). The developed method was validated by the standard Kjeldahl distillation/titration method for the analysis of milk and chicken meat samples. The proposed system had sample throughput of 35h(-1) and consumed much smaller amounts of chemical than the standard method (275mg vs 17.5g of NaOH per analysis, respectively).
开发了一种带有气体扩散分离的简单流动注射(FI)电导系统,用于测定牛奶和鸡肉中的凯氏氮(或蛋白质)。按照凯氏标准方法对样品进行消化,消化液稀释后直接注入由4M氢氧化钠组成的供体流中。在碱性介质中,铵转化为氨,氨透过聚四氟乙烯膜扩散并溶解在受体流(水)中。氨的离解导致受体溶液的电导发生变化,该变化与注入溶液中最初存在的铵浓度呈线性比例关系。制作了一个流通式电导池和一个放大电路,有助于提高电导检测系统的灵敏度。使用水暖特氟龙胶带作为气体扩散膜且不对系统进行恒温控制,获得了10 - 100mgL(-1) N - NH(4)范围内的线性校准曲线,检测限为1mgL(-1),精密度良好(50mgL(-1) N - NH(4)进行11次重复进样的相对标准偏差为0.3%)。通过标准凯氏蒸馏/滴定法对牛奶和鸡肉样品进行分析,验证了所开发的方法。所提出的系统样品通量为35h(-1),与标准方法相比消耗的化学试剂要少得多(每次分析分别消耗275mg与17.5g氢氧化钠)。