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目的寻找快速、简便、安全、准确的测定三叶青中硒含量的方法。方法以三叶青药材为材料,40%盐酸作为预还原剂和掩蔽剂,采用加热预消解与微波消解相结合的消解方式对三叶青样品进行消解处理,并利用氢化物-原子荧光光谱法对三叶青中硒含量进行测定。结果硒标准溶液浓度在0~20.0μg/L范围内与荧光强度值呈良好的线性关系,相关系数为0.9996,最低检出浓度为0.030μg/L,相对标准偏差在0.9%~2.0%之间,回收率为99.7%~100.8%,该方法与国家法相比,测定结果相近,测定时间缩短了3~4倍,且用40%盐酸代替具有安全隐患的铁氰化钾作为掩蔽剂。结论加热预消解-微波消解-原子荧光光度法具有操作简便、快速、安全、准确、干扰少等优点,是测定三叶青中硒含量的有效方法。
Objective To find a rapid, simple, safe and accurate method for the determination of selenium in clover leaf. Methods The clover green was taken as material, 40% hydrochloric acid was used as prereduction agent and masking agent. The digestion method was used to digest clover leaf samples by digestion with heating pre-digestion and microwave digestion. The hydride generation-atomic fluorescence spectrometry The content of selenium in selenium was determined. Results The concentration of selenium standard solution showed a good linear relationship with the fluorescence intensity in the range of 0 ~ 20.0μg / L with the correlation coefficient of 0.9996, the lowest detectable concentration of 0.030μg / L and the relative standard deviation of 0.9% ~ 2.0% , The recovery rate was 99.7% ~ 100.8%. Compared with the national method, the method was similar in determination results, and the measuring time was shortened by 3 to 4 times. Instead of the potential safety hazard of potassium ferricyanide as a masking agent, 40% hydrochloric acid was used. Conclusion Heating pre-digestion - microwave digestion - atomic fluorescence spectrophotometry has the advantages of simple, rapid, safe, accurate, less interference and is an effective method for the determination of selenium content in clover leaf.