超高效液相色谱-串联质谱法测定面制食品中十二烷基苯磺酸钠残留量  

Determination of Sodium Dodecyl Benzene Sulfonate Residues in Flour Foods by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄新望 张九魁 柯润辉[2] 王湛[1] 尹建军[2] 

机构地区：[1]北京工业大学环境与能源工程学院,北京100124 [2]中国食品发酵工业研究院国家食品质量监督检验中心,北京100015 [3]中国焙烤食品糖制品工业协会,北京100080

出　　处：《中国食品学报》2017年第12期251-257,共7页Journal of Chinese Institute Of Food Science and Technology

摘　　要：建立超高效液相色谱-串联质谱仪(UPLC-MS/MS)测定面制食品中十二烷基苯磺酸钠含量的新方法。将样品粉碎后,加入提取剂50%乙醇-水溶液、蛋白沉淀剂1 mol/L乙酸锌溶液和10.6%亚铁氰化钾溶液,超声提取,定容,微孔滤膜过滤,用LC-MS/MS进行定量分析。以Phenomenex Kintex C_(18)色谱柱为分析柱,甲醇-乙腈为流动相进行梯度洗脱,采用电喷雾电离源(ESI),以多反应监测(MRM)方式进行负离子检测。结果表明:十二烷基苯磺酸钠在0.5~20.0 mg/kg的范围内线性关系良好(R^2=0.9985),方法检出限为0.05 mg/kg,加标回收率在87.4%~96.8%之间,相对标准偏差≤4.5%,完全满足日常检测的要求。该方法前处理简单,测定快速、准确、灵敏度高,非常适合面制品中十二烷基苯磺酸钠的定量分析。An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric（UPLC-ESI-MS/MS） method was established for the determination of sodium dodecyl benzene sulfonate（SDBS） residues in flour foods. The sample preparation procedure involved an initial extraction of sample with 50% ethanol-water（V/V） solution,followed by adding 1 mol/L zinc acetate solution and 10.6% potassium ferrocyanide as protein precipitation solution. The extracts was filtered through 0.22 μm micropore filter and determinationed by UPLC-MS/MS. Phenomenex Kintex C18 column was used as the analytical column, and methanol-acetonitrile were used as mobile phase for gradient elution. Identification was achieved by electro spray ionization（ESI） in negative mode using multiple reaction monitoring（MRM）. The calibration curves were good linear between the peak areas and the concentrations of 0.520.0 mg/kg, and the correlation coefficients（R2） were greater than 0.99. The limits of detection（LOD） was 0.05 mg/kg. The average recoveries for the analysis of fortified samples were in the range of 87.4%96.8% and relative standard deviations（RSDs） were lower than4.5%, respectively. The results indicated that the proposed method is easier, faster, more sensitive, and suitable for the qualitative and quantitative confirmation of SDBS in flour products.

关 键 词：超高效液相色谱 串联质谱 面制食品 十二烷基苯磺酸钠 

分 类 号：O657.63[理学—分析化学] TS213.2[理学—化学]