摘要
目的通过优化比色法反应条件,建立比色分光光度法测定天花粉中二氧化硫的残留量。运用试剂盒法、比色法、顶空气相色谱法验证,探讨这3种方法测定结果的相关性。方法采用紫外分光光度法测定试验最佳吸收波长;利用响应面分析法对影响含量的因素进行优化,在单因素试验的基础上选取试验因素与水平,根据中心复合设计试验原理,采用四因素三水平的响应面分析法确定最佳比色法反应条件。结果确定最佳吸收波长为560 nm;最佳比色法反应条件:氨基磺酸铵溶液、氢氧化钠溶液、盐酸副玫瑰苯胺溶液用量分别为0.5、1.0、1.0 mL;反应时间为15 min。在该反应条件下,二氧化硫残留量在1.0~50.0μg与峰面积线性关系良好,r=0.9998;平均回收率为104.5%~105.3%,RSD为0.30%。结论该方法操作简便,重现性好,线性范围宽,可为天花粉及其相关加工产品中二氧化硫残留量的测定提供参考。
Objective To optimize the condition of colorimetric reaction and establish a spectrophotometric colorimetric method for the detection of sulfur dioxide residues in Trichosanthis Radix and to determine the correlation of these three methods, namely the reagent kit method, the colorimetric method, and the head space gas chromatography. Methods The optimal absorbing wavelength was determined by UV spectrophotometric. Response surface methodology was utilized to optimize factors which influenced the content of sulfur dioxide residues. According to central composition design principle, the optimal colorimetric process was conditioned by response surface analysis with 4 factors and 3 levels determined by single factor experiments. Results At a maximum absorption wavelength of 560 nm, we determined an optimal derivation condition： ammonium sulfamate solution 0.5 mL, sodium hydroxide solution 1.0 mL, pararosaniline hydrochloride solution 1.0 mL, and static reaction time 15 min. An excellent linear relationship at a detection range of 1.0 -- 50.0 pg was obtained with a correlation coffient of 0.9998, the average recovery rate of 104.5% -- 105.3%, and RSD of 0.30%. Conclusion The established method is easy to operate and shows a superior reproducibility and accuracy. It provids a reference for the determination of sulfur dioxide residues in Trichosanthis Radix and other related processed products.
出处
《中南药学》
CAS
2017年第4期505-510,共6页
Central South Pharmacy
基金
公益性中医药行业科研专项(No.201407003)
长沙市科技计划重点项目(No.k1406030-31)
湖南省重点学科药学学科资助
关键词
天花粉
二氧化硫残留量
比色法
试剂盒法
顶空气相色谱法
Trichosanthis Radix
residue of sulfur dioxide
colorimetry
reagent kit method
head space gas chromatography
