高效液相色谱法测定牛奶中双乙酸钠  

Determination of Sodium Diacetate in Milk by High performance Liquid Chromatography

作　　者：吴新[1] 包梦醒 余雯静[1] 郑利[1] 

机构地区：[1]苏州出入境检验检疫局,江苏苏州215104 [2]苏州产品质量监督检验所,江苏苏州215104

出　　处：《农产品加工（下）》2012年第10期143-145,153,共4页Farm Products Processing

摘　　要：建立了牛奶中双乙酸钠的快速测定方法,为执法提供技术支持。牛奶样品用水提取,加入硫酸锌溶液(0.5 mol/L)和氢氧化钾溶液(0.5 mol/L)沉淀、超声、离心,用C18柱分离,二极管阵列检测器测定,外标法定量。色谱条件:Agilent TC-C18色谱柱,流动相为质量浓度1.5 g/L磷酸氢二铵溶液与甲醇体积比为90:10,流速1mL/min。线性范围10～500μg/mL,相关系数R^2=0.99957,定量检测限50 mg/kg,空白样品添加50,100,500μg/mL 3个水平,回收率为101.12%～103.68%,相对标准偏差为2.01%～3.93%(n=6),说明方法准确可靠。A rapid determination method for sodium diacetate in milk is established to provide technical support for law enforcement. The milk samples are extracted with water, adding zinc sulfate solution （0.5 mol/L） , and potassium hydroxide solution （0.5 mol/L）. After precipitation, ultrasonic, centrifugation, then separated with a C18 column, determined by DAD detector and quantified by external standard. Chromatographic conditions： the Agilent TC-C18 column, mobile phase is 1.5 g/L of diammonium phosphate solution： methanol is 90 ： 10, flow rate is 1 mL/min. Experimental linear range is 10-500 ug/mL; correlation coefficient R2 = 0.999 57, quantitative detection limit is 50 mg/kg. Adding 50, 100 and 500 ug/mL levels to a blank sample, recoveries of 101.12%-103.68% and relative standard deviation in the range of 2.01%-3.93% （n=6） are finally gotten. This method is accurate and reliable for determination for sodium diacetate in milk.

关 键 词：牛奶 双乙酸钠 高效液相色谱法 

分 类 号：O657.72[理学—分析化学] TS252.7[理学—化学]