摘要
目的应用高效液相色谱法同时测定牛乳及乳粉中硝酸盐、亚硝酸盐和硫氰酸盐含量。方法采用ODS色谱柱,乙腈-0.05 mol/L磷酸二氢钾(含0.2%三乙胺,用磷酸调节pH3.3~3.4)(5+95)为流动相,流速1.0 ml/min,二极管阵列检测器检测,检测波长212 nm。结果三种化合物在0.5 mg/L^100.0 mg/L浓度范围内线性良好,牛乳及乳粉样品的最低检出浓度分别为:硝酸盐0.01 mg/L、0.2 mg/kg;亚硝酸盐0.02 mg/L、0.4 mg/kg;硫氰酸盐0.05 mg/L、1.0 mg/kg。相对标准偏差为1.5%~2.9%,回收率为92%~108%。结论该方法快速准确、灵敏简便,可以用于牛乳及乳粉中硝酸盐、亚硝酸盐和硫氰酸盐的检测。
Objective HPLC was applied to the determination of nitrate, nitrite and thiocyanate in milk and dry milk. Methods Prodigy 5 p.ODS3 column （250 mm ~ 4.6 mm） was used with a mixture of acetonitrile and 0.05 mol/L potassium dihydrogen phosphate （Containing 0.2% triethylamine solution, pH between 3.3 -3.4） as mobile phase at the ratio of 5 ＋ 95, the flow - rate was 1.0 ml/min. UV - detection at 212 nm with diode array detector （DAD） was adopted in the determination. Results The good linearity between peak area and concentration of all the 3 compounds were found in the range of 0.5 mg/L - 100.0 mg/L. The detection limits of milk and dry milk were 0.01 rag/L, 0.2 mg/kg for nitrate, 0.02 rag/L, 0.4 mg/kg for nitrite, 0.05 mg/L, 1.0 mg/kg for thiocyanate. The RSDs （n = 6） were in the range of 1.5% ~ 2.9% and the recovery were from 92% to 108%. Conclusion The method is rapid, accurate, sensitive, simple, it can be used for the determination of nitrate, nitrite and thiocyanate in milk and dry milk.
出处
《中国卫生检验杂志》
北大核心
2013年第15期3035-3037,共3页
Chinese Journal of Health Laboratory Technology
关键词
高效液相色谱法
牛乳及乳粉
硝酸盐
亚硝酸盐
硫氰酸盐
High performance liquid chromatography （HPLC）
Milk and dry milk
Nitrate
Nitrite
Thiocyanate
