优化比色法测定不同产地天花粉中二氧化硫残留量
|
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 μg 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.
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 μg 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.
引文
[1]马鸿雁,王媛媛,李运英.硫磺熏蒸加工中药材的研究进展[J].中药与临床,2015,6(1):54-57.
[2]Meng ZQ,Liu YX.Effects of sulfur dioxide inha-lation on ultrastructures of brains,hearts,kidneys and testicles from mice[J].Acta Scien Circum,2006,26(1):130-136.
[3]Paneliya AM.Antitussive activity of Vasa Avaleha formulations on sulfur dioxide-induced coughing in mice[J].Int J GN Pharm(IJGP),2015,9(3):180-183.
[4]Harsoliya MS,Patel VM,Singh S,et al.Anti tussive effect of multi uses medicinal plants on sulfur dioxide gas induced cough reflex in mice[J].J Pharm Res,2011,4(11):4123-4125.
[5]Meng Z.Oxidative damage of sulfur dioxide on various organs of mice:sulfur dioxide is a systemic oxidative damage agent[J].Inhal toxicol,2003,15(2):181-195.
[6]Zhang J,Liang C,Ma J,et al.Effects of sodium fluoride and sulfur dioxide on sperm motility and serum testosterone in male rats[J].Fluoride,2006,39(2):126-131.
[7]杨瑛,彭艳梅.市售10种中药饮片中二氧化硫残留量测定[J].湖南中医药大学学报,2012,32(1):38-39.
[8]Zhong Z,Li G,Zhu B,et al.A rapid distillation method coupled with ion chromatography for the determination of total sulphur dioxide in foods[J].Food Chem,2012,131(3):1044-1050.
[9]郏征伟,毛北萍,苗水,等.顶空气相色谱法测定硫黄熏蒸中药材中二氧化硫的残留量[J].药学学报,2014,49(2):277-281.
[10]杨文英,王芳.甲醛吸收-盐酸副玫瑰苯胺法测定食品中的亚硫酸盐[J].中国卫生检验杂志,2006,16(4):400-402.
[11]郭振忠,胡云峰,李文生,等.乙二胺四乙酸二钠-盐酸副玫瑰苯胺检测干果中二氧化硫的方法研究[J].食品科学,2009,30(8):247-250.
[12]薛艳.比色法快速测定党参中二氧化硫的残留量[J].安徽农业科学,2012,40(26):12859-12860.
[13]安宇,曹玉奇,孙雪楠,等.响应面分析优化荧光衍生法测定人参中二氧化硫残留量的研究[J].药物分析杂志,2015,35(1):84-92.
[14]杨文志,高宇,张引,等.盐酸副玫瑰苯胺法测定人参中二氧化硫残留含量的研究[J].人参研究,2014,26(2):23-25.
[15]郑平,陈开灯,陈功轩,等.干菜中二氧化硫残留量快速测定方法探究[J].广州化工,2013,41(12):135-137.
[16]中国药典2015年版.第四部新增补[S].2015:2331.
[2]Meng ZQ,Liu YX.Effects of sulfur dioxide inha-lation on ultrastructures of brains,hearts,kidneys and testicles from mice[J].Acta Scien Circum,2006,26(1):130-136.
[3]Paneliya AM.Antitussive activity of Vasa Avaleha formulations on sulfur dioxide-induced coughing in mice[J].Int J GN Pharm(IJGP),2015,9(3):180-183.
[4]Harsoliya MS,Patel VM,Singh S,et al.Anti tussive effect of multi uses medicinal plants on sulfur dioxide gas induced cough reflex in mice[J].J Pharm Res,2011,4(11):4123-4125.
[5]Meng Z.Oxidative damage of sulfur dioxide on various organs of mice:sulfur dioxide is a systemic oxidative damage agent[J].Inhal toxicol,2003,15(2):181-195.
[6]Zhang J,Liang C,Ma J,et al.Effects of sodium fluoride and sulfur dioxide on sperm motility and serum testosterone in male rats[J].Fluoride,2006,39(2):126-131.
[7]杨瑛,彭艳梅.市售10种中药饮片中二氧化硫残留量测定[J].湖南中医药大学学报,2012,32(1):38-39.
[8]Zhong Z,Li G,Zhu B,et al.A rapid distillation method coupled with ion chromatography for the determination of total sulphur dioxide in foods[J].Food Chem,2012,131(3):1044-1050.
[9]郏征伟,毛北萍,苗水,等.顶空气相色谱法测定硫黄熏蒸中药材中二氧化硫的残留量[J].药学学报,2014,49(2):277-281.
[10]杨文英,王芳.甲醛吸收-盐酸副玫瑰苯胺法测定食品中的亚硫酸盐[J].中国卫生检验杂志,2006,16(4):400-402.
[11]郭振忠,胡云峰,李文生,等.乙二胺四乙酸二钠-盐酸副玫瑰苯胺检测干果中二氧化硫的方法研究[J].食品科学,2009,30(8):247-250.
[12]薛艳.比色法快速测定党参中二氧化硫的残留量[J].安徽农业科学,2012,40(26):12859-12860.
[13]安宇,曹玉奇,孙雪楠,等.响应面分析优化荧光衍生法测定人参中二氧化硫残留量的研究[J].药物分析杂志,2015,35(1):84-92.
[14]杨文志,高宇,张引,等.盐酸副玫瑰苯胺法测定人参中二氧化硫残留含量的研究[J].人参研究,2014,26(2):23-25.
[15]郑平,陈开灯,陈功轩,等.干菜中二氧化硫残留量快速测定方法探究[J].广州化工,2013,41(12):135-137.
[16]中国药典2015年版.第四部新增补[S].2015:2331.