中药材二氧化硫快速定量检测系统的研发及验证

Development and verification of a rapid quantitative detection system for sulfur dioxide residues of Chinese herbal medicines

中文关键词:  中药材  二氧化硫  快速检测  定量

英文关键词:Chinese medicinal materials  sulfur dioxide  rapid detection  quantitative

中文摘要:

      目的 建立一种针对中药材二氧化硫残留特异性强的定量快速检测系统。方法 利用醋酸铅检测微量硫化氢的高敏感性, 设计以硫化铅黑色沉淀的灰度响应值为定量依据的醋酸铅检测卡, 及可控制反应条件使硫化铅灰度可线性地反映二氧化硫含量的检测反应器, 研发与检测卡配套的可准确检测灰度值的定量检测仪。制备标准灰度卡、绘制检测灰度值与标准溶液浓度关系曲线、考察定量检测系统的精密度、加样回收率、时间稳定性, 同时做干扰实验及用本系统与国标方法对同一批次中药材的二氧化硫残留量进行检测比较, 评价检测体系的定量检测效果。结果 本检测系统试纸条的灰度值与二氧化硫标准溶液的浓度线性关系良好(r2=0.99), 线性检测范围为0~805 mg/kg; 对高中低浓度的二氧化硫残留样品多次检测值的相对标准偏差均小于5%, 加样回收率达到85%以上, 准确性良好; 常见的含硫化合物对其没有干扰, 本检测系统与2015版药典第三法(离子色谱法)对同一批次的中药材二氧化硫检测结果一致。结论 该检测系统准确性好, 稳定可靠, 特异性强, 操作简便, 可用于中药材二氧化硫残留的快速定量检测。

英文摘要:

      Objective To establish a quantitative and rapid detection system of sulfur dioxide residues in Chinese herbal medicines. Methods Based on the high sensitivity of lead acetate to detect trace hydrogen sulfide, the lead acetate detection card based on the gray scale response value of lead sulfide black precipitation was designed, the detection reactor with controlled reaction conditions was designed to linearly reflect the sulfur dioxide content of lead sulfide, and the quantitative detector which can accurately detect the gray value was developed with the detection card. The standard gray card was propagated, the detection of grey value and the standard solution concentration curve were drawn, and the precision, sample recoveries and time stability of the quantitative detection system were investigated. At the same time, the interference experiment was carried out and the SO2 residues in the same batch of Chinese medicinal materials were detected and compared with the system and the national standard method to evaluate the quantitative detection effect of the detection system. Results The gray value of the test strip of this detection system had a good linear relationship with the concentration of the standard solution (r2=0.99), and the linear detection range was 0-805 mg/kg. The relative standard deviation of the sulfur dioxide residual samples with high, medium and low concentrations were less than 5%, and the recovery rates were more than 85% with good accuracy. Common sulfur compounds had no interference with it, and the detection system was consistent with the detection results of sulfur dioxide for the same batch of Chinese herbal medicines by the third method (ion chromatography) in 2015 edition of pharmacopoeia. Conclusion The system is accurate, stable, reliable, specific and easy to operate, which is suitable for rapid quantitative determination of sulfur dioxide residues in Chinese medicinal materials.