摘要
目的：建立应用超声萃取反相离子对高效液相色谱法测定食品中亚硝酸盐和硝酸盐含量的方法。方法：食品样品经温水浴，超声萃取，去脂肪和沉淀蛋白后，进样20出，以甲醇-混合磷酸盐（1．25mmol／L Na2HPO4和1．25mmol／L KH2PO4及内含4mmol／L四丁基溴化铵）（体积比为20：80）为流动相，流速为1．0ml／min，经Gemini^TM C18色谱柱（250×4．6mm，5μm）柱分离，225nm检测。结果：亚硝酸盐、硝酸盐完全分离，R〉1．5，在0．20～100．00mg／L范围内成线性，相关系数大于0．9995，检出下限分别为0．08，0．10mg／L，回收率在97．4％～101．9％之间。结论：该方法准确、灵敏，操作简便，同时测定硝酸盐和亚硝酸盐，适合于食品样品中硝酸盐和亚硝酸盐的测定。
Objective：A rapid and simple ultrasonic extraction ion-pair reversed-phase high performance liquid chromato-graphic method （HPLC） has been established for routine analysis of nitrite and nitrate in foods. Methods： Sample of foods was extracted with ultrasonic in warm water,and removed protein and fat,then detected by HPLC. The HPLC analysis conditions were： chromatographic column Gemini^TM C18 （250 × 4. 6 mm,5μm）, detecting wavelength 225 nm, the ratio of mobile phase methanol-phosphate buffer （ 1.25 mmol/L disodium hydrogen phosphate, 1.25 mmol/L potassium dihydrogen phosphate） that contains 4 mmol/L tetrabutylammonium bromide （V/V） was 80/20, flowing rate 1.0 ml/min, injected sample volume 20 μl. Results, The resolution factor of nitrite and nitrate was more than 1.5. Calibration curves were linear for two analytes at 0.30-100.0 mg/L and the correlation coefficient was more than 0.9995. The detection limits for nitrite and nitrate were 0.08 mg/L and 0.10 mg/ L Overall recoveries were between 97.4% and 101.9%. Conclusion：The method is sensitive, accurate, convenient and quick, which can be used to simultaneously detect nitrite and nitrate residues in foods.
出处
《中国卫生检验杂志》
CAS
2007年第12期2151-2152,2190,共3页
Chinese Journal of Health Laboratory Technology
关键词
离子对反相高效液相色谱法
亚硝酸盐
硝酸盐
超声萃取
Ion-pair reversed-phase high performance liquid chromatographic
Nitrite
Nitrate
Ultrasonic extraction
