uplc-msms法测定奶粉中烟酸的含量 determination of nicotinic acid in milk powder by ultra performance liquid chromatography-tandem mass spectrometry.pdfVIP

UPLC-MS/MS法测定奶粉中烟酸的 含量 1 2 1 文 ∕郝 刚 俞蕴莉 顾炳仁 （1江苏省苏州市食品药品检验所；2江苏省苏州大学附属第二医院） 摘　要：建立一种专属、灵敏、快速的超高效液相色谱串联质谱（UPLC-MS/MS）测定奶粉中烟酸含量的方法。烟酸提 取后经强阳离子交换（SCX）固相萃取柱净化，采用BEH-C18超高效液相色谱柱、20 mmol/L乙酸水溶液—乙腈（体积比为 20∶80）流动相分离，以电喷雾离子源正离子方式进行多反应监测（MRM）。试验结果表明，1～500 ng/L浓度范围内，烟 酸呈良好的线性关系，相关系数R=0.9995。低、中、高3 个烟酸浓度添加水平的回收率为78.2%～90.4%，相对标准偏差小 于7%。奶粉中烟酸的检出限为0.25 µg/g，定量限为0.75µg/g。采用所建方法对市售6 批奶粉进行测定，烟酸含量均符合规 定。所建方法适合奶粉中烟酸的含量测定。　　 关键词：超高效液相色谱串联质谱；奶粉；烟酸 Determination of Nicotinic Acid in Milk Powder by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry HAO Gang1 YU Yun-li2 GU Bing-ren1 ， ， 1 Suzhou Institute for Food and Drug Control 2 The Second Affiliated Hospital of Soochow University （ ； ） Abstract: A specific, sensitive and rapid method is presented for the determination of nicotinic acid in milk powder by ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS . Nicotinic acid in the test samples was extracted （ ） and cleaned-up with a strong cation exchange SCX column and analysed by UPLC-MS/MS. Nicotinic acid was separated by （ ） a BEH-C18 UPLC column and 20 mmol/L ammonium acetate – acetonitrile 20 80, v/v as mobile phase, and electrospray （ ∶ ） ionization was applied and operated in the positive ion mode by MRM. The calibration curves showed good linear relationship in the range of 1 500 ng/mL for nicotinic acid with the correlation coefficient of 0.9995. The average recoveries of nicotinic acid in milk ～ powder samples at the three concentrations ranged from 78.2% to 90.4% with the relative standard deviations less than 7%. The limit of detection LOD and limit of quantification LQD of nicotinic acid w