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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

发布时间:2019-01-12 19:56
【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。
[Abstract]:A new method for the determination of sodium dodecylbenzene sulfonate in noodle food by ultra-high performance liquid chromatography-tandem mass spectrometer (UPLC-MS/MS) was established. After the sample was pulverized, 50% ethanol aqueous solution, 1 mol/L zinc acetate solution and 10.6% potassium ferrocyanide solution were added as extractant, then ultrasonic extraction, constant volume filtration, micropore filtration and quantitative analysis by LC-MS/MS. Phenomenex Kintex C _ (18) column was used as analytical column, methanol-acetonitrile was used as mobile phase for gradient elution, and (ESI), was used as electrospray ionization source to detect negative ions by multi-reaction monitoring (MRM). The results showed that the linear range of sodium dodecylbenzenesulfonate was 0.5 ~ 20.0 mg/kg (R ~ (2 +) 0.9985), the detection limit of the method was 0. 05 mg/kg, and the recovery rate was between 87. 4% and 96. 8%. Relative standard deviation 鈮,

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