摘要
收集朱砂生产加工工艺流程中不同工艺点的样品，采用仿生提取-电感耦合等离子体发射原子光谱法（仿生提取-ICP-OES法）对朱砂样品中可溶性重金属含量进行测定。研究结果表明：仿生提取-ICP-OES法能满足13种重金属同时检测要求，13种重金属线性范围均在0.1-1000.0μg/L之间，线性相关系数为0.9901-1.0000，检出限为0.0893-16.0414μg/L；该方法重复性相对标准偏差DRS均小于10.0%，精密度的DRS均小于7.1%，加样回收率为83.0%-117.5%，满足检测要求；在工艺流程中，朱砂的可溶性重金属含量呈逐步降低趋势，参照《药用植物及制剂进出口绿色行业标准》的限量标准，仅有H-5的Cd超出标准及H-3，H-4和H-5样品的Pb超出标准；仿生提取-ICP-OES法简单、快速，准确性及精度高，能够通过同时检测朱砂加工工艺过程中13种可溶性重金属含量检测，为实时监控朱砂加工工艺质量提供参考依据，有助于完善并确定最佳的朱砂生产加工流程。
Cinnabar samples with different processes in production and processing process were collected. Soluble heavy metals in cinnabaris were determined in the process of production and processing by inductively coupled plasma- optical emission spectrometry（ICP-OES） with bionic extraction and microwave digestion technology. The results show that 13 kinds of elements have excellent linearity over the range of 0.1-1 000.0 μg/L with a correlation coefficient of 0.990 1-1.000 0. Limits of detection are in the range of 0.089 3-16.041 4 μg/L. Relative standard deviation DRS of the repeatability is less than 10.0%. DRS of precision is lower than 7.1%. Spike recoveries in the range of 83.0%-117.5% are obtained. In the process, the content of soluble heavy metals＇ gradually reduces. With reference to green trade standards of importing ＆ exporting medicinal plants ＆ preparations, none of the samples surpass the legal limit for Cd in H-5 and Pb in H-3, H-4 and H-5. The bionic extraction-ICP-OES method is simple and fast, and it has high accuracy and high precision. This method provides reference for real-timely monitoring process quality with simultaneously detecting cinnabaris＇ 13 kinds of soluble heavy metals in machining process. The method can help improve and determine the best cinnabaris＇ production and processing processes.
出处
《中南大学学报（自然科学版）》
EI
CAS
CSCD
北大核心
2016年第11期3658-3663,共6页
Journal of Central South University:Science and Technology
基金
国家科技部十二五专项(2014ZX09304-307)~~
