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目的:建立应用2,4-二硝基苯肼衍生化和毛细管柱气相色谱-电子捕获检测器测定腐竹中甲醛次硫酸氢钠的方法。方法:试样经氯化钠-盐酸溶液回旋振荡提取、2,4-二硝基苯肼衍生化后,用正已烷萃取衍生产物,经毛细管柱色谱分离、电子捕获检测器测定,外标峰面积定量。结果:方法检出限为0.12μg/kg(S/N=10)。加标平均回收率为94.2%～96.4%,相对标准偏差为5.4%～6.4%(n=6),峰面积与浓度在0.2μg/ml～3.2μg/ml范围内呈良好的线性关系,相关系数为0.9999。结论:该方法灵敏度高、准确、快速,适合批量腐竹中甲醛次硫酸氢钠的测定。
OBJECTIVE: To establish a method for the determination of sodium formaldehyde sulfoxylate in yuba by using 2,4-dinitrophenylhydrazine derivatization and capillary gas chromatography-electron capture detector. Methods: The sample was extracted by rotary shaker with sodium chloride-hydrochloric acid solution and derivatized with 2,4-dinitrophenylhydrazine. The derivatized product was extracted with n-hexane, separated by capillary column chromatography, determined by electron capture detector, Peak area quantitative. Results: The detection limit was 0.12 μg / kg (S / N = 10). The average recoveries were 94.2% ~ 96.4% and the relative standard deviations were 5.4% ~ 6.4% (n = 6). The peak area was linear with the concentration ranging from 0.2μg / ml to 3.2μg / ml The coefficient is 0.9999. Conclusion: The method is sensitive, accurate and rapid and suitable for the determination of formaldehyde sodium sulfoxylate in bulk yuba.