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机构地区:[1]河北化工医药职业技术学院,河北石家庄050026
出 处:《安徽农业科学》2009年第13期5823-5824,共2页Journal of Anhui Agricultural Sciences
摘 要:[目的]探索高效液相色谱法测定熟肉制品中苯甲酸和山梨酸含量的方法。[方法]将苯甲酸和山梨酸经氢氧化钠溶液浸泡后,经蛋白质沉淀和过滤,被测组分滞留于水相中与杂质分离。取相同体积样液和苯甲酸和山梨酸标准溶液分别注入液相色谱仪进行分析。[结果]加入20%硫酸铜溶液10 ml并放置40 min能较好的盐析蛋白质。甲醇含量为5%时有较好的分离度和合适的保留时间,流动相甲醇与0.02 mol/L醋酸铵配比为5∶95,流速为1.0 ml/min时,苯甲酸与山梨酸的色谱分离较好。苯甲酸、山梨酸的保留时间分别为5.6457、.736 min,相对标准偏差分别为1.63%和3.99%;平均回收率分别为86.8%和91.6%;最小检出量分别为1.0、0.5 ng。[结论]采用该方法沉淀完全,检出限低,预处理较简便,损失少,线性好。[Objective] The study aimed to discuss the method of determining benzoic acid and sorbic acid content in the cooked meat products by HPLC. [ Method] Benzoic acid and sorbic acid were soaked in sodium hydroxide liquor, after sedimentation and filtration of protein, the tested components were detained in water phrase and separated from impurity. The sample liquid and standard liquid of benzoic acid and sorbic acid with same volume were injected into the liquid chromatography for analysis. [ Result] The better salted out protein could be got when 10 ml 20% copper sulfate liquid was added into sample solution and it was kept stationary for 40 min. When the content of methanol was 5 %, it had better resolution and suitable retention time. When the ratio of methanol to 0.02 mel/L ammonium acetate in mebile phrase was 5:95 and the flow rate was 1.0 ml/min, the chromalographic separation of benzoic acid and sorbic acid was better. The retention time of benzoic acid and sorbic acid was 5.645 and 7.736 min resp., their relative standard deviation was 1.63% and 3.99% resp., their average recovery was 86.8% and 91.6% resp. and their minimum detectable quantity was 1.0 and 0.5 ng resp. [Conclusion] This method proved to be complete in precipitation, low in detection limit, simple in pretreatment, few in loss and good in linearity.
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