差示扫描量热法对5种硫酸盐类矿物药的分析鉴别研究
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摘要
目的:采用差示扫描量热法(differential scanning calorimetry,DSC)对芒硝、生石膏、玄明粉、白矾及寒水石等5种硫酸盐类矿物药进行分析鉴别,以探讨DSC法快速鉴别硫酸盐类矿物药的可行性。方法:收集不同来源的芒硝、生石膏、玄明粉、白矾及寒水石,共30批样品,考察升温范围、升温速率2个因素对DSC的影响,并在最佳条件下通过DSC图谱区分5种硫酸盐类矿物药。结果:升温范围30～400℃,升温速率40℃/min为DSC法快速鉴别5种硫酸盐类矿物药的最佳条件。芒硝有4个明显吸热峰,峰形拐点分别为(41±1)、(111±4)、(219±4)及(255±1)℃;生石膏有2个明显特征峰,(185±3)℃为吸热峰温,(381±2)℃为放热峰温;玄明粉有2个明显吸热峰,峰形拐点分别为(227±5)、(257±2)℃,与芒硝后2个峰接近;白矾有3个明显吸热峰,峰形拐点分别为(100±1)、(121±2)及(249±1)℃;寒水石在400℃范围内无明显特征峰。结论:DSC法具有操作简便、测量快速、重现性好、谱图易解析和样品用量少等优点,可快速鉴别硫酸盐类矿物药。
OBJECTIVE: To analyze and identify five kinds of sulfate minerals including natrii sulfas, gypsum fibrosum, natrii sulfas exsiccatus, alumen and calcitum by differential scanning calorimetry(DSC), so as to investigate the feasibility of DSC method for rapid identification of sulfates mineral drugs. METHODS: Natrii sulfas, gypsum fibrosum, natrii sulfas exsiccatus, alumen and calcitum from different sources were collected. A total of 30 batches of samples were investigated. The effects of temperature scope and heating rate on DSC experiments were investigated. Five kinds of sulfate minerals were distinguished by DSC. RESULTS: Temperature range of 30 to 400 ℃, the heating rate of 40 ℃/min for DSC method to identify the best condition of five kinds of sulfate mineral drugs. There were four obvious endothermic peaks in natrii sulfas, and the peak inflection points were(41±1),(111±4),(219±4) and(255±1)℃. Gypsum fibrosum had two distinct characteristic peaks,(185±3)℃ was the endothermic peak temperature,(381±2)℃ was the exothermic peak temperature. Natrii sulfas exsiccatus had two obvious endothermic peaks, the peak shape inflection point was(227±5),(257±2)℃, which was close to the two peaks of natrii sulfas. There were three obvious endothermic peaks in alumen, the peak inflection points were(100±1),(121±2) and(249±1)℃, respectively. Calcitum had no obvious characteristic peak in the range of 400 ℃. CONCLUSIONS: The DSC method has the advantages of simple operation, rapid measurement, good reproducibility, easy analysis of spectra and low sample consumption, and can quickly identify sulfate minerals.
OBJECTIVE: To analyze and identify five kinds of sulfate minerals including natrii sulfas, gypsum fibrosum, natrii sulfas exsiccatus, alumen and calcitum by differential scanning calorimetry(DSC), so as to investigate the feasibility of DSC method for rapid identification of sulfates mineral drugs. METHODS: Natrii sulfas, gypsum fibrosum, natrii sulfas exsiccatus, alumen and calcitum from different sources were collected. A total of 30 batches of samples were investigated. The effects of temperature scope and heating rate on DSC experiments were investigated. Five kinds of sulfate minerals were distinguished by DSC. RESULTS: Temperature range of 30 to 400 ℃, the heating rate of 40 ℃/min for DSC method to identify the best condition of five kinds of sulfate mineral drugs. There were four obvious endothermic peaks in natrii sulfas, and the peak inflection points were(41±1),(111±4),(219±4) and(255±1)℃. Gypsum fibrosum had two distinct characteristic peaks,(185±3)℃ was the endothermic peak temperature,(381±2)℃ was the exothermic peak temperature. Natrii sulfas exsiccatus had two obvious endothermic peaks, the peak shape inflection point was(227±5),(257±2)℃, which was close to the two peaks of natrii sulfas. There were three obvious endothermic peaks in alumen, the peak inflection points were(100±1),(121±2) and(249±1)℃, respectively. Calcitum had no obvious characteristic peak in the range of 400 ℃. CONCLUSIONS: The DSC method has the advantages of simple operation, rapid measurement, good reproducibility, easy analysis of spectra and low sample consumption, and can quickly identify sulfate minerals.
引文
[1] 国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:127.
[2] 高学敏.中药学[M].北京:中国中医药出版社,2017:158.
[3] 国家中医药管理局《中华本草》编委会.中华本草蒙药卷[M].上海:上海科学技术出版社,2004:55-56.
[4] 张钦德.中药鉴定技术[M].北京:人民卫生出版社,2005:194.
[5] 李晓明,邵爱娟,陈敏,等.生、煅石膏的粉晶X-射线衍射分析[J].中国实验方剂学杂志2010,16(17):75-78.
[6] 刘元芬,李祥,高锦飚,等.石膏炮制前后红外光谱分析特征鉴定[J].内蒙古中医药,2007,26(5):27-29.
[7] 明晶,陈龙,陈科力,等.白矾、硼砂等6种白色结晶矿物药鉴别[J].中国实验方剂学杂志,2016,22(20):33-38.
[8] 朱晓静,李峰,王集会,等.芒硝和玄明粉的X射线粉末衍射鉴别比较[J].山东中医杂志,2013,32(4):280.
[9] 仇紫璇.热分析技术在药品检验中的应用[J].中西医结合心血管病杂志,2018,6(23):40-41.
[10] Hassa-Roudsari M,Goff HD.A new quantitative method to measure activity of ice structuring proteins using differential scanning calo-rimetry[J].Cryo Letters,2012,33(2):118-125.
[11] 张超,赵晓燕,马越,等.使用差示扫描量热仪测定抗冻蛋白热滞活性方法的研究[J].生物物理学报,2008,24(6):465-473.
[12] 刘圣金,杨欢,徐春祥,等.TG-DSC分析法在矿物药禹余粮质量控制中的应用[J].中药材,2016,39(1):121-123.
[13] 喻喜华,陈晓辉,李泽运,等.山茱萸及其伪品的差示扫描量热法鉴别[J].中成药,2011,33(7):1197-1198.
[14] 殷学毅.阿胶、龟甲胶、鹿角胶的热分析区分鉴定[J].湖北中医药大学学报,2013,15(2):39-41.
[15] 张丽,郭永辉,侯艳艳,等.差示扫描量热法与红外光谱法快速鉴别肉苁蓉药材的对比研究[J].医药导报,2014,33(3):360-363.
[16] 陈佳,李明华,余坤子,等.差示扫描量热法用于珍珠粉与贝壳粉真伪鉴别的研究[J].中国中药杂志,2015,40(8):1459-1462.
[17] Zhang C,Zhang H,Wang L.Effect of carrot(Daucus carota)antifreeze proteins on the fermentation capacity of frozen dough[J].Food Res Int,2007,40(6):763-769.
[2] 高学敏.中药学[M].北京:中国中医药出版社,2017:158.
[3] 国家中医药管理局《中华本草》编委会.中华本草蒙药卷[M].上海:上海科学技术出版社,2004:55-56.
[4] 张钦德.中药鉴定技术[M].北京:人民卫生出版社,2005:194.
[5] 李晓明,邵爱娟,陈敏,等.生、煅石膏的粉晶X-射线衍射分析[J].中国实验方剂学杂志2010,16(17):75-78.
[6] 刘元芬,李祥,高锦飚,等.石膏炮制前后红外光谱分析特征鉴定[J].内蒙古中医药,2007,26(5):27-29.
[7] 明晶,陈龙,陈科力,等.白矾、硼砂等6种白色结晶矿物药鉴别[J].中国实验方剂学杂志,2016,22(20):33-38.
[8] 朱晓静,李峰,王集会,等.芒硝和玄明粉的X射线粉末衍射鉴别比较[J].山东中医杂志,2013,32(4):280.
[9] 仇紫璇.热分析技术在药品检验中的应用[J].中西医结合心血管病杂志,2018,6(23):40-41.
[10] Hassa-Roudsari M,Goff HD.A new quantitative method to measure activity of ice structuring proteins using differential scanning calo-rimetry[J].Cryo Letters,2012,33(2):118-125.
[11] 张超,赵晓燕,马越,等.使用差示扫描量热仪测定抗冻蛋白热滞活性方法的研究[J].生物物理学报,2008,24(6):465-473.
[12] 刘圣金,杨欢,徐春祥,等.TG-DSC分析法在矿物药禹余粮质量控制中的应用[J].中药材,2016,39(1):121-123.
[13] 喻喜华,陈晓辉,李泽运,等.山茱萸及其伪品的差示扫描量热法鉴别[J].中成药,2011,33(7):1197-1198.
[14] 殷学毅.阿胶、龟甲胶、鹿角胶的热分析区分鉴定[J].湖北中医药大学学报,2013,15(2):39-41.
[15] 张丽,郭永辉,侯艳艳,等.差示扫描量热法与红外光谱法快速鉴别肉苁蓉药材的对比研究[J].医药导报,2014,33(3):360-363.
[16] 陈佳,李明华,余坤子,等.差示扫描量热法用于珍珠粉与贝壳粉真伪鉴别的研究[J].中国中药杂志,2015,40(8):1459-1462.
[17] Zhang C,Zhang H,Wang L.Effect of carrot(Daucus carota)antifreeze proteins on the fermentation capacity of frozen dough[J].Food Res Int,2007,40(6):763-769.