文献类型：期刊文献

中文题名：响应面分析优化荧光衍生法测定硫熏党参及其饮片二氧化硫残留量的研究

英文题名：Optimization of Fluorescence Derivative Method for Determination of Sulfur Dioxide Residues in Sulfur-fumigated Dangshen and Its Decoction Pieces by Response Surface Analysis

作者：远俊洋[1,2];李端[1,2];侯嘉[1];邵士俊[2];杨扶德[1]

第一作者：远俊洋

机构：[1]甘肃中医药大学药学院,甘肃兰州730000;[2]中国科学院兰州化学物理研究所,甘肃兰州730000

第一机构：甘肃中医药大学药学院（西北中藏药协同创新中心办公室）

年份：2020

卷号：41

期号：9

起止页码：210

中文期刊名：食品工业科技

外文期刊名：Science and Technology of Food Industry

收录：CSTPCD;;北大核心:【北大核心2017】；

基金：科技部国家重点研发计划项目(2018YFC1706305);国家自然科学基金项目(81360622);甘肃省省属普通本科高校基本科研业务费专项资金(甘财教[2014]63号-5);兰州市2014年人才创新创业专项(2014-2-15);甘肃省高等学校科研项目(2014B-055)。

语种：中文

中文关键词：加工炮制;荧光衍生法;响应面优化;硫熏时间;二氧化硫残留

外文关键词：processing;fluorescence derivatization;response surface optimization;sulfur fumigration time;sulfur dioxide residue

摘要：将党参样品分别硫熏0、30、60、90 min,并加工炮制为节子货、厚片、米炒、蜜制四个规格的饮片,对不同硫熏时间党参及其饮片SO 2残留量进行研究。通过单因素实验及响应面优化试验确定最佳衍生条件为:缓冲溶液pH为6.6,缓冲溶液用量为1.5 mL,邻苯二甲醛用量为2.1 mL,乙酸铵浓度为2.5 mmol/L,乙酸铵用量为2.0 mL,反应温度、反应时间和静置时间分别为50℃、5 min及40 min,在此条件下测得平均荧光强度为955865.21。荧光衍生法方法考察结果显示:亚硫酸钠浓度在0.01~0.2μg/mL之间,其荧光强度有较好的线性关系,检测限为1.89×10^-3μg/mL;精密度、稳定性、重复性RSD分别为:0.76%、4.13%和1.59%,平均回收率98.61%,RSD为4.89%,且专属性考察结果较好。荧光衍生法可作为党参SO2残留量测定的方法,其测得结果与酸碱滴定法测定结果相比平均高24.87%。SO2残留量测定结果表明:党参硫熏0、30 min原药材SO2残留量未超出药典标准,而硫熏60、90 min原药材SO2残留量超出药典标准;硫熏党参经加工炮制后,饮片较原药材SO 2残留量明显降低,蜜制饮片SO2残留量最低。
The samples of dangshen were fumigated with sulfur for 0,30,60,90 min,and processed into four sizes,sections,flakes,stir-frying with rice and honey,to determine the SO 2 residue of dangshen and its decoction pieces in different sulphur time.By single-factor experiments and response surface optimization experiments,the optimal derivation conditions were determined as follows:pH of the buffer solution was 6.6,the dosage of buffer solution was 1.5 mL,and the amount of o-phthalaldehyde was 2.1 mL.The concentration of ammonium acetate was 2.5 mmol/L,the dosage of ammonium acetate was 2.0 mL,the reaction temperature was 50℃,the reaction time was 5 min,and the static reaction time was 40 min,and the average fluorescence intensity measured under these conditions was 955865.21.The results of the fluorescence derivatization method showed that the concentration of sodium sulfite was between 0.01 and 0.2μg/mL,and the fluorescence intensity had a good linear relationship.The detection limit was 1.89×10^-3μg/mL.The precision,stability,and repeatability RSD were 0.76%,4.13%,and 1.59%,the average recovery was 98.61%,and the RSD was 4.89%.The results of specific surveys were better.It could be used as a method for the determination of SO2 residue in dangshen,and the measured results were 24.87% higher than those measured by acid-base titration on average.The measurement results showed that the SO2 residues of the dangshen original medicinal in fumigated with sulfur for 0 and 30 min did not exceed the standards of Chinese Pharmacopoeia,and sulfur fumigation of the original medicinal material SO2 residues for 60 and 90 min exceeded the standards.After processing of sulfur dangshen,the residual amount of SO2 in the decoction pieces was significantly lower than that of the original medicinal materials,and the SO2 residue in the decoction pieces of honey was the lowest.