熊果苷对照品的定值研究
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摘要
目的:联合质量平衡法、差示扫描量热法及定量核磁共振法3种定值方法测定熊果苷对照品的纯度。方法:首先,采用高效液相色谱法和气相色谱法测定熊果苷对照品的色谱纯度,采用卡尔费休库伦法、电感耦合等离子体质谱法、顶空气相色谱法分别测定其水分、灰分和残留溶剂,由质量平衡法计算熊果苷对照品的纯度;其次,采用差示扫描量热法对熊果苷对照品纯度加以验证;最后,以定量核磁共振法测定其绝对纯度。结果:质量平衡法和差示扫描量热法定值结果经科克伦法判定互为等精度,取其算术平均值作为最终定值结果,即熊果苷对照品纯度为99.12%,RSD为0.029%;定量核磁共振法测定结果为99.12%,RSD为0.036%。结论:质量平衡法、差示扫描量热法及定量核磁共振法对熊果苷对照品的定值结果基本一致,3种方法能够更好地保证熊果苷对照品赋值的准确性。
Objective:To determine the content of arbutin by the three methods including mass balance,differential scanning calorimetry(DSC)and quantitative nuclear magnetic resonance(qNMR). Methods:Firstly,the chromatographic purity of arbutin reference substance was determined by HPLC & GC methods. Moisture,ignition residue and residual solvents were determined by Karl-Fischer-Coulomb method,inductively coupled with plasma mass spectrometry and headspace gas chromatography,respectively. The purity of arbutin reference substance was calculated by mass balance method. Secondly,the purity of arbutin reference substance was verified by differential scanning calorimetry. Finally,the absolute purity of arbutin reference substance was determined by qNMR. Results:The results of mass balance method and differential scanning calorimetry were of equal precision by Cochran test. Thus,the arithmetic average value was 99.12% with RSD of 0.029%,which was taken as the final content of arbutin reference substance. And the result of qNMR was 99.12% with RSD of 0.036%. Conclusion:The assignment results of mass balance,differential scanning calorimetry and qNMR were consistent,and three methods can guarantee the accuracy of the assignment.
Objective:To determine the content of arbutin by the three methods including mass balance,differential scanning calorimetry(DSC)and quantitative nuclear magnetic resonance(qNMR). Methods:Firstly,the chromatographic purity of arbutin reference substance was determined by HPLC & GC methods. Moisture,ignition residue and residual solvents were determined by Karl-Fischer-Coulomb method,inductively coupled with plasma mass spectrometry and headspace gas chromatography,respectively. The purity of arbutin reference substance was calculated by mass balance method. Secondly,the purity of arbutin reference substance was verified by differential scanning calorimetry. Finally,the absolute purity of arbutin reference substance was determined by qNMR. Results:The results of mass balance method and differential scanning calorimetry were of equal precision by Cochran test. Thus,the arithmetic average value was 99.12% with RSD of 0.029%,which was taken as the final content of arbutin reference substance. And the result of qNMR was 99.12% with RSD of 0.036%. Conclusion:The assignment results of mass balance,differential scanning calorimetry and qNMR were consistent,and three methods can guarantee the accuracy of the assignment.
引文
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[2]王亚芳,周宇娜,张建军.熊果苷镇咳、祛痰及平喘的药效学研究[J].中草药,2003,34(8):739WANG YF,ZHOU YN,ZHANG JJ. Pharmacodynamics study on antitussive,expectorant and antiasthmatic effects of arbutin[J].Chin Tradit Herb Drugs,2003,34(8):739
[3]王佩,赖瑛,吴锡铭.熊果苷抗炎作用的研究[J].中华中医药学刊,2008,6(9):1933WANG P,LAI Y,WU XM. Study on anti-inflammatory effect of arbutin[J]. Chin Arch Tradit Chin Med,2008,6(9):1933
[4]王佩,赖瑛,吴锡铭.熊果苷与甘草酸合用对免疫性炎症的治疗作用[J].中国中医药信息杂志,2009,16(1):31WANG P,LAI Y,WU XM. Therapeutic effect of combination of arbutin and glycyrrhizin on immune inflammation[J]. Chin J Inf Tradit Chin Med,2009,16(1):31
[5]LIM YJ,LEE EH,KANG TH,et al. Inhibitory effects of arbutinon melanin biosynthesis of alpha-melanocyte stimulating hormoneinduced hyperpigmentation in cultured brownish guinea pig skin tissues[J]. Arch Pharm Res,2009,32(3):367
[6]孙竞阳,冯中华,侯熙彦,等.熊果苷类似物的合成、表征及美白活性[J].中国药物化学杂志,2017,27(4):267SUN JY,FENG ZH,HOU XY,et al. Synthesis,characterization and whitening activity of arbutin analogues[J]. Chin J Med Chem,2017,27(4):267
[7]刘彩云,吴培诚,梁高卫,等. 3种熊果苷的研究进展[J].日用化学工业,2015,45(9):529LIU CY,WU PC,LIANG GW,et al. Progress in development of three kinds of arbutin product[J]. China Surfact Deterg Cosmet,2015,45(9):529
[8]房军,杜顺晶,金银龙.熊果苷在化妆品中应用的研究进展[J].卫生研究,2009,38(1):111FANG J,DU SJ,JIN YL. Research progress of arbutin in cosmetics[J]. J Hyg Res,2009,38(1):111
[9]马玲云,常艳,戴忠,等.基于多元数据分析研究葛根素化学对照品定值准确性与其影响因素的相关性[J].药物分析杂志,2013,33(12):2156MA LY,CHANG Y,DAI Z,et al. Correlation between the calibration accuracy of puerarin and its influential factors based on multivariate analysis[J]. Chin J Pharm Anal,2013,33(12):2156
[10]吴昊,刘斌,王伟,等.荷叶的化学对照品2-羟基-1-甲氧基阿朴啡研究[J].药物分析杂志,2010,30(9):1650WU H,LIU B,WANG W,et al. Lotus leaf chemical reference substance 2-hydroxy-1-methoxy apomorphine study[J]. Chin J Pharm Anal,2010,30(9):1650
[11]郑新元,张茉,王杰,等.黄芩苷对照品2种定值方法比较研究[J].药物分析杂志,2014,34(6):1130ZHENG XY,ZHANG M,WANG J,et al. A comparison study on two measuring methods of baicalin reference substance[J]. Chin J Pharm Anal,2014,34(6):1130
[12]徐敏,陈智群,王民昌,等. NTO纯度标准物质定值研究[J].化学分析计量,2011,20(3):4XU M,CHEN ZQ,WANG MC,et al. NTO purity reference material study[J]. Chem Anal Meter,2011,20(3):4
[13]张海波,李新霞,孟磊,等.蒜氨酸标准物质的定值研究[J].食品科学,2014,35(12):80ZHANG HB,LI XX,MENG L,et al. Study on the value of alliin reference materials[J]. Food Sci,2014,35(12):80
[14]马康,苏福海,王海峰,等.有机纯度标准物质定值技术研究进展[J].分析测试学报,2013,32(7):901MA K,SU FH,WANG HF,et al. Progress on certified technique for chemical purity of organic reference material[J]. J Instrum Anal,2013,32(7):901
[15]黄亮,张伟,黄挺,等.肌酐纯度标准物质的定值方法及其不确定度评定研究[J].分析测试学报,2014,33(7):840HUANG L,ZHANG W,HUANG T,et al. Research on a certified reference material for purity of creatinine and its uncertainty evaluation[J]. J Instrum Anal,2014,33(7):840
[16]张凤兰,苏哲,吴景,等.β-熊果苷和氢醌安全性评价及化妆品法规管理现状[J].环境与健康杂志,2017,34(11):1017ZHANG FL,SU Z,WU J,et al. Safety assessment ofβ-arbutin and hydroquinone and current situation of cosmetics regulation management[J]. J Environ Health,2017,34(11):1017