电感耦合等离子体质谱法测定白酒中铅的前处理方法

Pretreatment method for determination of lead in liquor by inductively coupled plasma mass spectrometry

中文关键词:  白酒  铅  电感耦合等离子体质谱法  直接酸化稀释法  蒸干乙醇酸化稀释法  微波消解法

英文关键词:liquor  lead  inductively coupled plasma mass spectrometry  direct acidification dilution method  evaporated ethanol acidification dilution method  microwave digestion method

中文摘要:

      目的 探讨不同前处理方法对使用电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)测定白酒中铅含量检测结果准确性的影响。方法 采用直接酸化稀释法、蒸干乙醇酸化稀释法和微波消解法分别对3份白酒样品及质控白酒样品进行前处理, 使用10 μg/L铋溶液作为在线内标, 使用ICP-MS得到标准工作曲线后, 测定白酒中的铅含量, 并进行回收率实验。结果 标准物质和加标回收率情况表明直接酸化稀释法处理的白酒样品铅平均含量偏低一些, 但与其他2种方法相比差异不显著(P＞0.05)。3种前处理方法对质控样品测定结果都在允许误差范围内。直接酸化稀释法存在一定的基体影响, 蒸干乙醇酸化稀释法和微波消解法稳定性更好。结论 蒸干乙醇酸化稀释法简化了白酒样品的前处理过程, 减少了硝酸的用量, 结果可靠, 可在今后的检测工作中进行使用。

英文摘要:

      Objective To explore the influence of different pretreatment methods on the accuracy of the determination results of lead in liquor by inductively coupled plasma mass spectrometry (ICP-MS). Methods Three liquor samples and quality control liquor sample were pretreated by direct acidification dilution method, evaporated alcohol acidification dilution method and microwave digestion method respectively and 10 μg/L bismuth solution was used as internal standard online. After getting the standard working curve by ICP-MS, the content of lead in liquor was determined and the recovery test was carried out. Results The recovery rate of reference material and standard addition showed that the average lead content of liquor samples treated by direct acidification dilution method was lower than that of the other two methods, but the difference was not significant. The results of the 3 pretreatment methods were all within the allowable error range. The direct acidification dilution method had certain matrix effect, and the stability of the evaporation dry ethanol acidification dilution method and microwave digestion method were better. Conclusion The evaporative dry ethanol dilution method simplifies the pretreatment process of liquor samples and reduces the amount of nitric acid. The results of this method are reliable and this method can be used in future testing work.