CAJ | 학술논문

研究建立利用加压毛细管电色谱（pCEC）测定乳及乳制品中三聚氰胺的分析方法。样品采用2%三氯乙酸水溶液超声提取，阳离子固相萃取柱（MCX）净化，提取液经C18反相毛细管电色谱柱分离，流动相乙腈-10 mmol/L辛烷磺酸钠溶液（pH 3.0）=15+85，泵流速0.05 mL/min，分离电压-2 kV，紫外检测器240 nm检测。该方法在1.0 mg/kg~100 mg/kg质量浓度范围内线性关系良好（R2=0.999），在牛奶和酸奶中的定量限为2.5 mg/kg，在奶粉中的定量限为10 mg/kg，加标回收率为78.9%～93.5%，相对标准偏差小于5%。
연구건립이용가압모세관전색보（pCEC）측정유급유제품중삼취청알적분석방법。양품채용2%삼록을산수용액초성제취，양리자고상췌취주（MCX）정화，제취액경C18반상모세관전색보주분리，류동상을정-10 mmol/L신완광산납용액（pH 3.0）=15+85，빙류속0.05 mL/min，분리전압-2 kV，자외검측기240 nm검측。해방법재1.0 mg/kg~100 mg/kg질량농도범위내선성관계량호（R2=0.999），재우내화산내중적정량한위2.5 mg/kg，재내분중적정량한위10 mg/kg，가표회수솔위78.9%～93.5%，상대표준편차소우5%。
An effective and convenient method for determination of melamine in milk and dairy product was developed. Pressurized capillary electro-chromatography (pCEC) was used as separation technology. The samples were extracted by ultrasonic with 2 % trichloroacetic acid solution , cleaned up by mixed cation exchange solid phase extraction (MCX SPE). The separation was performed on a reversed phase C18 column with 240 nm as the UV detection wavelength. The mobile phase was composed of acetonitrile and sodium octanesulfonate solution (15∶85, v/v, pH3.0), at a pump flow rate of 0.05 mL/min and separation voltage of-2 kV. Under the optimal conditions, the linear range of melamine was 1.0 mg/kg-100 mg/kg with correlation coefficient higher than 0.999. The LOQ was 2.5 mg/kg in milk and yoghurt , and 10 mg/kg in milk powder. The recoveries were 78.9%-93.5%and the relative standard deviations (RSD) were less than 5%.