湿法回流消解-氢化物-原子荧光光谱法测定 营养强化剂中总硒含量

Determination of total selenium in selenium nutrition enhancer by refluxing wet digestion-hydride generation-atomic fluorescence spectrometry

中文关键词:  富硒营养强化剂  总硒  氢化物-原子荧光光谱法

英文关键词:selenium nutrition enhancer  total selenium  hydride generation-atomic fluorescence spectrometry (HG-AFS)

中文摘要:

      目的 建立湿法回流消解-氢化物-原子荧光光谱法测定营养强化剂中总硒的含量。方法 采用硝酸-高氯酸(4:1, V:V)作为消解体系230 ℃回流消解, 采用氢化物-原子荧光光谱法进行测定; 并考查消解体系、还原剂和掩蔽剂等对荧光强度的影响。结果 采用4.0%盐酸作为酸介质, 硼氢化钾浓度为2.0%时荧光强度最强。硒在浓度范围为2.0~40.0 ng/mL呈现良好的线性关系, 相关系数为0.9999, 方法检出限为0.028 ng/mL, 加标回收率为93.0%~102.0%, 相对标准偏差为2.2%(n=6)。结论 该方法试剂用量少、消解速度快、准确度好、灵敏度高, 适合于富硒营养强化剂中总硒含量的测定。

英文摘要:

      Objective To establish a method for the determination of total selenium in nutrition enhancer by hydride generation-atomic fluorescence spectrometry (HG-AFS) with refluxing wet digestion．Methods The nitric acid-perchloric acid (4:1, V:V) was used as the digestion system with reflux digestion temperature of 230 ℃. Samples were detected by the method of hydride generation-atomic fluorescence spectrometry. And then the effects of digestion system, reducing agent and masking agent on fluorescence intensity were investigated. Results The fluorescence intensity was the strongest using 4.0% hydrochloric acid as acid medium and 2.0% potassium borohydride. Selenium had a good linear relationship in the range of 2.0~40.0 ng/mL with the correlation coefficient of 0.9999. The limit of detection was 0.028 ng/mL. The recovery rates at 3 spiked levels were in the range of 93.0%~102.0%, and RSD was 2.2% (n=6)．Conclusion This method is simple, rapid, and accurate, and reliable for the determination of total selenium in selenium nutrition enhancer．