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作 者:陈东宇[1] 汤晓艳[1] 孙京新[2] 王敏[1] 金芬[1] 毛雪飞[1]
机构地区:[1]中国农业科学院农业质量标准与检测技术研究所,农业部农产品质量安全重点实验室,北京100081 [2]青岛农业大学,山东青岛266109
出 处:《食品科学》2013年第2期148-151,共4页Food Science
基 金:"十二五"国家科技支撑计划项目(2012BAD28B03);"十一五"国家科技支撑计划项目(2009BADB7B07);国家自然科学基金青年科学基金项目(3 1000799)
摘 要:建立一种用离色谱法同步检测生鲜肉消毒残留的二氧化氯(ClO_2)及其降解副产物亚氯酸根(ClO_2^-)、氯酸根(ClO_3^-)含量。样品经0.05mol/L的磷酸盐缓冲液(pH4.3)-乙腈(50:50,V/V)提取,向离心后的上清液中加过量的亚硝酸根(NO_2^-)反应,氢氧化钙溶液调节pH值至7~8,并沉淀杂质离子,正己烷除脂,采用AS11-HC色谱柱分离,15mmol/L KOH溶液以1.0mL/min流速等度淋洗,电导检测器检测,外标法定量。本方法得出ClO_2、ClO_2^-、ClO_3^-的最低检出限分别为0.5、0.7、0.5mg/L,定量限分别为1.0、1.2、1.0mg/L。结果表明利用IC法检测生鲜肉中ClO_2、ClO_2^-、ClO_3^-含量,方法准确、可靠、实用性强。Abstract: An analytical method was developed to simultaneously determine chlorine dioxide (C102) and its degradation byproducts chlorite (CIO2) and chlorate (CIO3) in fresh meat by ion chromatography (IC). Samples were extracted with 0.05 mol/L phosphate buffer-acetonitrile solution (pH 4.3, 50:50, V/V), and the centrifugal supernatant was then added with an excess amount of NO2 and adjusted to pH 7-8 with calcium hydroxide solution to precipitate unwanted ions. After defatting with n-hexane, the chromatographic separation was performed on an AS11-HC column through isocratic elution using 15 mmol/L KOH solution at a flow rate of 1.0 ml.Jmin. The analytes were detected using a conductivity detector and quantified by external standard method. The limits of detection (LOD) and limit of quantification (LOQ) of the IC method were 0.5 mg/L and 1.0 mg/L, 0.7 mg/L and 1.2mg/L, and 0.5 mg/L and 1.0 mg/L for C102, CIO2 and C103, respectively. This method was accurate, reliable and practical.
关 键 词:离子色谱法 生鲜肉 CLO2 ClO2- ClO3-
分 类 号:TS207.3[轻工技术与工程—食品科学]
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