UPLC-MS/MS测定小麦粉及其制品与小麦粉添加剂中新型非法添加物乙酰氧肟酸

Determination of New Illegal Additives Acetohydroxamic acid in Wheat Flour and its Products and Wheat Flour Additives by UPLC-MS/MS

摘要:

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定小麦粉及其制品与小麦粉添加剂中新型非法添加物乙酰氧肟酸的分析方法。方法选取小麦粉、小麦粉添加剂、面皮、面条、馒头等5种具有代表性的样品为研究基质，以甲醇为提取溶剂，经超声和涡旋振荡提取，高速离心、过滤，通过T3色谱柱(100 mm × 3.0 mm，2.7 μm)分离，以0.1%甲酸溶液和甲醇作为洗脱流动相，采用大气压化学电离源、多反应监测模式检测，外标法定量。结果表明，乙酰氧肟酸的溶剂和基质标准曲线在0.075 ~ 5.00 mg/L范围内线性关系良好，相关系数均大于0.999，检出限为0.25 mg/kg，加标回收率为78.49% ~ 108.61%，相对标准偏差（RSD，n=6）为1.67% ~ 7.50%。该方法抗干扰能力强，准确度高，适用于小麦粉及其制品与小麦粉添加剂中乙酰氧肟酸的测定。

Abstract:

An analytical method of new illegal additives acetohydroxamic acid(AHA) in wheat flour and its products and wheat flour additives was developed by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Five representative samples of wheat flour, wheat flour additive, flour crust, noodles and steamed bread were selected as the research matrix. Methanol was used as the extraction solvent. After ultrasonic and vortex oscillation, high-speed centrifugation and filtration, the separation was performed on T3 column (100 mm × 3.0 mm,2.7 μm) using 0.1% aqueous formic acid and methanol. The detection was used by atmospheric pressure chemical ionization source(APCI), multi-reaction monitoring mode, and quantified by external standard method. The results showed that the solvent and matrix standard curves of AHA had a good linear relationship in the concentration range of 0.075 ~ 5.00 mg/L with correlation coefficients of higher than 0.999. The limits of detection(LOD) was 0.25 mg/kg. The recoveries were in the range of 78.49% ~ 108.61% with the relative standard deviation(RSD,n=6) of 1.67% ~ 7.50%. The method had strong anti-interference ability and high accuracy. It can meet the identification and quantification of AHA in wheat flour and its products and wheat flour additives.