矿物药白矾、枯矾及其伪品的SEM,XRD鉴别分析
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摘要
目的:铵明矾为白矾的常见伪品,铵明矾炮制品为枯矾的常见伪品,该文旨在建立鉴别白矾、枯矾、铵明矾及其炮制品的方法。方法:利用扫描电子显微镜及X射线衍射技术对样品进行分析。结果:白矾、铵明矾在炮制前后形貌特征变化明显。白矾、铵明矾在×250,×1 000倍数下均能显示明显的形貌差异。白矾呈不规则的碎片或碎块,边缘棱角清晰,表面较平滑,散有不规则块小颗粒,偶见孔洞和纵棱;铵明矾呈不规则团块状,边缘较钝圆,棱角不明显,表面多凹凸不平,散有较小、呈类圆形的小颗粒。枯矾及伪品枯矾在×250倍数下,两者形貌特征区分度不大,在×1 000倍数下,枯矾表面凹凸不平,呈明显的粗颗粒状,伪品枯矾表面较平坦,粗颗粒状特征不明显。通过粉晶X射线衍射,能快速、准确的鉴别白矾、枯矾、铵明矾、铵明矾炮制品的主要物相为KAl(SO4)2·12H2O,NH4Al(SO4)2·12H2O,KAl(SO4)2,NH4Al(SO4)2,X射线衍射峰2θ角度特征值分别为23,12,22,5个。结论:扫描电子显微镜及X射线衍射技术均可用于白矾、枯矾及其相应伪品的鉴别。
Objective: Ammonium alum is a common counterfeit of Alumen,and the processed product of ammonium alum is a common counterfeits of calcined Alumen. This paper aims to establish a method for identifying Alumen, calcined Alumen, ammonium alum and their processed products. Method: The samples were analyzed by scanning electron microscope(SEM) and X ray diffraction(XRD) in this paper. Result:Ammonium alum and Alumen showed obvious changes in morphology after processing. Both Alumen and ammonium alum showed obvious differences in morphology at × 250 and × 1 000 times microscope. Alumen presented irregular fragments,clear edge corners,smooth surface,scattered irregular small particles,occasional holes and longitudinal edges. Ammonium alum presented irregular clumps,blunt edges,not obvious edges and corners,uneven surface,scattered smaller and round-like particles. The difference in morphology was not obvious at × 250 times microscope between Alumen and ammonium alum processed products. While at × 1 000 times,the surface of calcined Alumen was uneven with coarse particles; the surface of counterfeit calcined Alumen was flat,and the coarse particle characteristics were not obvious. XRD can be used to rapidly and accurately identify the primary phase of Alumen,calcined Alumen,ammonium alum and ammonium alum processed products: KAl(SO4)2·12 H2 O,NH4 Al(SO4)2·12 H2 O,KAl(SO4)2,and NH4 Al(SO4)2 respectively,with 2θ angle characteristic value of 23,12,22 and 5 respectively for XRD peak. Conclusion: SEM and XRD techniques can be used for the identification of Alumen,calcined Alumen,ammonium alum and their counterfeit products.
Objective: Ammonium alum is a common counterfeit of Alumen,and the processed product of ammonium alum is a common counterfeits of calcined Alumen. This paper aims to establish a method for identifying Alumen, calcined Alumen, ammonium alum and their processed products. Method: The samples were analyzed by scanning electron microscope(SEM) and X ray diffraction(XRD) in this paper. Result:Ammonium alum and Alumen showed obvious changes in morphology after processing. Both Alumen and ammonium alum showed obvious differences in morphology at × 250 and × 1 000 times microscope. Alumen presented irregular fragments,clear edge corners,smooth surface,scattered irregular small particles,occasional holes and longitudinal edges. Ammonium alum presented irregular clumps,blunt edges,not obvious edges and corners,uneven surface,scattered smaller and round-like particles. The difference in morphology was not obvious at × 250 times microscope between Alumen and ammonium alum processed products. While at × 1 000 times,the surface of calcined Alumen was uneven with coarse particles; the surface of counterfeit calcined Alumen was flat,and the coarse particle characteristics were not obvious. XRD can be used to rapidly and accurately identify the primary phase of Alumen,calcined Alumen,ammonium alum and ammonium alum processed products: KAl(SO4)2·12 H2 O,NH4 Al(SO4)2·12 H2 O,KAl(SO4)2,and NH4 Al(SO4)2 respectively,with 2θ angle characteristic value of 23,12,22 and 5 respectively for XRD peak. Conclusion: SEM and XRD techniques can be used for the identification of Alumen,calcined Alumen,ammonium alum and their counterfeit products.
引文
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[7]尤淑霞,吴德康,刘圣金,等.白矾的炮制研究概况[J].中药材,2010,33(7):1192-1194.
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[10]乔婷婷,刘圣金,林瑞超,等.基于ICP-OES/MS技术的白矾及其伪品铵明矾的无机元素差异性分析[J].中药材,2016,39(11):2462-2468.
[11]尤淑霞,刘圣金,吴德康,等.白矾和枯矾的FTIR指纹图谱比较研究[J].药物分析杂志,2011,31(6):1054-1058.
[12]包贝华,刘圣金,姚卫峰,等.傅里叶变换红外分光光度法鉴别白矾及枯矾的实验研究[J].药物分析杂志,2010,30(6):1148-1151.
[13]杨柳,王薇,梁惟俊,等.不同产地石膏的扫描电镜观察[J].中国药师,2015,18(2):326-328.
[14]张慧,高岩,熊慧,等.采用扫描电镜能谱仪比较水飞法水洗法及干研法对雄黄饮片质量的影响[J].中国实验方剂学杂志,2018,24(11):22-26.
[15]刘芳,郑义蕾,王霄,等.基于红外光谱和扫描电镜的川贝母粉末掺杂鉴别研究[J].南京中医药大学学报,2017,33(4):417-419.
[16]明小芳,尚祥伟,张超,等.纳米雄黄酸水飞品X射线衍射及拉曼光谱分析[J].中国实验方剂学杂志,2018,24(20):89-94.
[17]刘圣金,吴德康,林瑞超,等.矿物类中药青礞石的XRD Fourier指纹图谱研究[J].中国中药杂志,2011,36(18):2498-2502.
[18]杨欢,刘圣金,吴德康,等.矿物药禹余粮X射线衍射Fourier指纹图谱研究[J].药物分析杂志,2014,34(12):2171-2180.
[19]房方,李祥,刘圣金,等.矿物中药钟乳石的X射线衍射Fourier指纹图谱[J].光谱实验室,2013,30(5):2586-2590.
[2]江苏新医学院.中药大辞典.上册[M].上海:上海人民出版社,1977:1383.
[3]国家药典委员会.中华人民共和国药典.一部[M].北京:人民卫生出版社,1977:107-108.
[4]尤淑霞,吴德康,刘圣金,等.白矾的基原考证及药理作用[J].中国中医药信息杂志,2010,17(7):111-112.
[5]尤淑霞.白矾及炮制品品质评价研究[D].南京:南京中医药大学,2011.
[6]黄依雯,刘圣金,高丽丽.枯矾的临床应用研究进展[J].中国药房,2010,21(11):1043-1044.
[7]尤淑霞,吴德康,刘圣金,等.白矾的炮制研究概况[J].中药材,2010,33(7):1192-1194.
[8]刘圣金,吴德康,孔德平.矿物类中药白矾的炮制工艺研究进展[J].中国药房,2009,20(36):2870-2871.
[9]林瑞超.矿物药检测技术与质量控制[M].北京:科学出版社,2013:693.
[10]乔婷婷,刘圣金,林瑞超,等.基于ICP-OES/MS技术的白矾及其伪品铵明矾的无机元素差异性分析[J].中药材,2016,39(11):2462-2468.
[11]尤淑霞,刘圣金,吴德康,等.白矾和枯矾的FTIR指纹图谱比较研究[J].药物分析杂志,2011,31(6):1054-1058.
[12]包贝华,刘圣金,姚卫峰,等.傅里叶变换红外分光光度法鉴别白矾及枯矾的实验研究[J].药物分析杂志,2010,30(6):1148-1151.
[13]杨柳,王薇,梁惟俊,等.不同产地石膏的扫描电镜观察[J].中国药师,2015,18(2):326-328.
[14]张慧,高岩,熊慧,等.采用扫描电镜能谱仪比较水飞法水洗法及干研法对雄黄饮片质量的影响[J].中国实验方剂学杂志,2018,24(11):22-26.
[15]刘芳,郑义蕾,王霄,等.基于红外光谱和扫描电镜的川贝母粉末掺杂鉴别研究[J].南京中医药大学学报,2017,33(4):417-419.
[16]明小芳,尚祥伟,张超,等.纳米雄黄酸水飞品X射线衍射及拉曼光谱分析[J].中国实验方剂学杂志,2018,24(20):89-94.
[17]刘圣金,吴德康,林瑞超,等.矿物类中药青礞石的XRD Fourier指纹图谱研究[J].中国中药杂志,2011,36(18):2498-2502.
[18]杨欢,刘圣金,吴德康,等.矿物药禹余粮X射线衍射Fourier指纹图谱研究[J].药物分析杂志,2014,34(12):2171-2180.
[19]房方,李祥,刘圣金,等.矿物中药钟乳石的X射线衍射Fourier指纹图谱[J].光谱实验室,2013,30(5):2586-2590.