甘氨酸max (L.)中丙泊尼残留分析方法的改进Merrill和Pisum sativum .的脱蛋白工艺

H. Ham, J. Choi, J. Hur
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引用次数: 0

摘要

背景:二硫代氨基甲酸酯杀菌剂丙泊尼可采用衍生化反应-高效液相色谱/紫外分光光度法进行定量分析,重现性和稳定性高。然而,大豆和豌豆中高蛋白的存在影响了衍生过程,导致极低的回收率。因此,本研究采用氯仿-凝胶法脱蛋白工艺,改进大豆和豌豆中丙泊尼的分析方法。方法与结果:用50 mL氯仿对大豆和豌豆分别进行6次和5次脱蛋白。经过4次脱蛋白,再与碘化甲酯衍生化反应,两种脉冲对丙炔的回收率均大于90%。但当脱蛋白次数大于5次时,回收率有下降的趋势。方法定量限(LOQ)为0.04 mg/L。10倍和50倍定量回收率为87.2 ~ 95.0%,变异系数<10%。结论(S):本研究证实,在高蛋白质含量的豆类中衍生分析二硫代氨基甲酸酯类杀菌剂时,采用氯仿凝胶法进行4次脱蛋白处理是有效的。然而,根据豆类中存在的初始蛋白质含量,回收率有所不同:蛋白质含量越低,丙炔的回收率越高。该方法有望用于去除农业样品中高含量的蛋白质分析干扰物。
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Improvement of Analytical Method for Propineb Residues in Glycine max (L.) Merrill and Pisum sativum L. using Deproteinization Process
BACKGROUND: Dithiocarbamate fungicide propineb can be analyzed quantitatively by derivatization reaction followed by HPLC/UVD, which has high reproducibility and stability. However, the presence of high protein in soybeans and peas affects the derivatization process re-sulting in extremely low recoveries. Therefore, this study was conducted to improve the analytical method for analysis of propineb in soybeans and peas by applying a deproteinization process using chloroform-gel method. METHODS AND RESULTS: The deproteinization process was carried out up to 6 times for soybeans and 5 times for peas using 50 mL chloroform. After 4 times of deproteinization process followed by a derivatization reaction with methyl iodide, the recovery yields of propineb in both pulses were >90%. However, the recovery yield tended to decrease when the deproteinization process was performed more than 5 times. The method limit of quantification (LOQ) was 0.04 mg/L. The recovery conducted in triplicate at 10 times and 50 times of the LOQ ranged from 87.2 to 95.0 % with a coefficient of variation <10%. CONCLUSION(S): This study confirmed that 4 times of deproteinization process using the chloroform-gel method was effective when derivatizing and analyzing dithiocarbamate fungicides in pulses with high protein content. However, depending on the initial protein content present in the pulses, there was a difference in the recovery: the lower the protein content, the higher the recovery rate of propineb. It is expected that the method proposed in this study could be applied to remove high content of protein as analytical interference substance from agricultural samples.
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