以普洱茶7542为参考样本,乙醇为溶剂,超声提取制备普洱茶醇溶物,建立了普洱茶7542醇溶物气相色谱-质谱(GC-MS)指纹图谱,同时对其指纹图谱进行相似度计算和主成分分析.试验结果表明,普洱茶醇溶物的最佳提取方法:采用50 mL 95%乙醇超声提...以普洱茶7542为参考样本,乙醇为溶剂,超声提取制备普洱茶醇溶物,建立了普洱茶7542醇溶物气相色谱-质谱(GC-MS)指纹图谱,同时对其指纹图谱进行相似度计算和主成分分析.试验结果表明,普洱茶醇溶物的最佳提取方法:采用50 mL 95%乙醇超声提取30 min,顶空进样最佳条件为振荡箱温度110℃,振荡时间20 min.通过对9个不同年限、不同批次的普洱茶7542系列样品醇溶物挥发性成分GC-MS指纹图谱进行相似度分析,测定样品醇溶物挥发性成分图谱与对照图谱之间的相似度在0.706~0.906之间,说明不同年限、不同批次的9个普洱茶7542醇溶物挥发性成分和参照样本相比发生了改变,但变化较小,但其共有成分峰面积百分含量存在差异.通过对9个不同年限、不同批次普洱茶7542醇溶物挥发性成分共有成分进行主成分分析,提取了2个成分,即2-羟甲基-2-甲基-吡咯烷-1-甲醛和N-丁基苯磺酰胺,其特征值大于1,累计方差贡献率达90.2%,能较好的代表9个不同年限、不同批次普洱茶7542的全部信息,可以用主成分分析来反映样品的全部信息.因此可通过测定9个不同年限、不同批次普洱茶7542醇溶物中2-羟甲基-2-甲基-吡咯烷-1-甲醛和N-丁基苯磺酰胺的含量差异评价普洱茶7542的质量.展开更多
目的:建立枳壳药材挥发油的气相色谱-质谱(GC-MS)指纹图谱。方法:采用GC-MS法,色谱柱为RTX-5MS毛细管柱,进样口温度为250℃,载气为高纯氦气(≥99.999%),流速为1.0 m L/min,分流比为10∶1,进样量为1μL(程序升温);采用电子轰击离子源,离...目的:建立枳壳药材挥发油的气相色谱-质谱(GC-MS)指纹图谱。方法:采用GC-MS法,色谱柱为RTX-5MS毛细管柱,进样口温度为250℃,载气为高纯氦气(≥99.999%),流速为1.0 m L/min,分流比为10∶1,进样量为1μL(程序升温);采用电子轰击离子源,离子源温度为230℃,检测器温度为250℃,溶剂延迟时间为3 min,扫描范围为m/z 35~550。以月桂烯为参照,测定21批药材挥发油样品的GC-MS图谱,采用《中药色谱指纹图谱相似度评价系统》(2004 A版)进行相似度评价,确定共有峰,采用LC Solution 2质谱库(NIST05.LIB和NIST05s.LIB)确定共有峰成分,并采用面积归一化法测定共有峰的相对含量。结果:21批药材挥发油样品的GC-MS图谱有20个共有峰,相似度均>0.90;经验证,21批药材挥发油样品GC-MS图谱与对照指纹图谱具有较好的一致性。枳壳药材挥发油主要成分为柠檬烯、萜品烯、月桂烯和D-Cadinene。结论:所建指纹图谱可为枳壳药材挥发油的真伪鉴别和质量评价提供参考。展开更多
Disulfide bond formation protein A （DsbA） is one of the important helper proteins for folding in protein synthesis in vivo. In this study, purification of recombinant DsbA was investigated by examining four importan...Disulfide bond formation protein A （DsbA） is one of the important helper proteins for folding in protein synthesis in vivo. In this study, purification of recombinant DsbA was investigated by examining four important factors with Box-Behnken design method, a statistic-based design of experiments. The optimal operation conditions were obtained by adopting the effectiveness coefficient method on the multi-objective problem, which takes the protein recovery, purification efficiency and throughput of ion-exchange chromatography into account. After the optimization, protein recovery of 96.8% and purity higher than 95% DsbA was achieved, and the productivity was （377.9±1.7） mg soluble DsbA per liter broth. The purified protein was identified by peptide mass fingerprinting matching the record of gil2624856, a mutant of DsbA. The DsbA was preliminarily applied to the refolding of denatured lysozyme in vitro.展开更多
A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed a...A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.展开更多
The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was devel...The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was developed for the quality control of the rhizomes of A.officinarum.Its chemical fingerprint was established using raw material of 15 different origins in China.Similarity analysis(SA)and hierarchical clusting analysis(HCA)were applied to select the qualitative markers.Principal components analysis(PCA)was conducted to select the quantitative markers of the rhizomes of A.officinarum samples from different origins.The constituents were confirmed by(+)electrospray ionization LC-MS.12 constituents were selected as common peaks and 10 of them were confirmed by(+)electrospray ionization LC-MS.Six bioactive constituents including DPHA,galangin flavanone,galangin,galangin 3-methylether,DPHB and DPHC were simultaneous determination by using the HPLC-DAD analysis.The developed method was able to determine the bioactive components with excellent resolution,precision and recovery.The results indicated that chromatographic fingerprint combination with multi-components determination method is suitable for quality assessment of the rhizomes of A.officinarum.展开更多
文摘以普洱茶7542为参考样本,乙醇为溶剂,超声提取制备普洱茶醇溶物,建立了普洱茶7542醇溶物气相色谱-质谱(GC-MS)指纹图谱,同时对其指纹图谱进行相似度计算和主成分分析.试验结果表明,普洱茶醇溶物的最佳提取方法:采用50 mL 95%乙醇超声提取30 min,顶空进样最佳条件为振荡箱温度110℃,振荡时间20 min.通过对9个不同年限、不同批次的普洱茶7542系列样品醇溶物挥发性成分GC-MS指纹图谱进行相似度分析,测定样品醇溶物挥发性成分图谱与对照图谱之间的相似度在0.706~0.906之间,说明不同年限、不同批次的9个普洱茶7542醇溶物挥发性成分和参照样本相比发生了改变,但变化较小,但其共有成分峰面积百分含量存在差异.通过对9个不同年限、不同批次普洱茶7542醇溶物挥发性成分共有成分进行主成分分析,提取了2个成分,即2-羟甲基-2-甲基-吡咯烷-1-甲醛和N-丁基苯磺酰胺,其特征值大于1,累计方差贡献率达90.2%,能较好的代表9个不同年限、不同批次普洱茶7542的全部信息,可以用主成分分析来反映样品的全部信息.因此可通过测定9个不同年限、不同批次普洱茶7542醇溶物中2-羟甲基-2-甲基-吡咯烷-1-甲醛和N-丁基苯磺酰胺的含量差异评价普洱茶7542的质量.
基金Supported by the National Natural Science Foundation of China （21036005）.
文摘Disulfide bond formation protein A （DsbA） is one of the important helper proteins for folding in protein synthesis in vivo. In this study, purification of recombinant DsbA was investigated by examining four important factors with Box-Behnken design method, a statistic-based design of experiments. The optimal operation conditions were obtained by adopting the effectiveness coefficient method on the multi-objective problem, which takes the protein recovery, purification efficiency and throughput of ion-exchange chromatography into account. After the optimization, protein recovery of 96.8% and purity higher than 95% DsbA was achieved, and the productivity was （377.9±1.7） mg soluble DsbA per liter broth. The purified protein was identified by peptide mass fingerprinting matching the record of gil2624856, a mutant of DsbA. The DsbA was preliminarily applied to the refolding of denatured lysozyme in vitro.
基金National Natural Science Foundation of China (Grant No.21372015 and 20872006)
文摘A simple, sensible and reliable HPLC-DAD fingerprint analysis method for the raw materials of Oxytropisfalcata and Oxytropis chiliophylla, both of which were used as ＂Er-Da-Xia＂ in Tibetan medicines, was developed and then subsequently applied to analyze samples collected from different locations or times. 19 common fingerprint peaks for O. falcata, 24 for O. chiliophylla, and 11 for the two herbs were designated respectively, including 7 identified characteristic peaks existing in both herbs and 1 uniquely presenting in O. chiliophylla. Although there were some slight differences in the chemicals of O. falcata and O. chiliophylla, the main components of both herbs were consistent generally. The results provided scientific basis, at least from the chemical point of view, for the reasonablity of two herbs being used as the same drug in Tibetan medicines and for the necessary of further investigation on their detailed chemical and pharmacological differences.
基金The National Natural Science Foundation of China(Grant No.81503210)the Medical Scientific Research Foundation of Guangdong Province(Grant No.B2017049)the Natural Science Foundation of Guangdong Food and Drug Vocational College(Grant No.2016YZ003)
文摘The rhizome of Alpinia officinarum Hance is a well-known traditional Chinese medicine(TCM)and has been widely used for the remedy of gastrointestinal diseases.In the present study,a simple and rapid HPLC-DAD was developed for the quality control of the rhizomes of A.officinarum.Its chemical fingerprint was established using raw material of 15 different origins in China.Similarity analysis(SA)and hierarchical clusting analysis(HCA)were applied to select the qualitative markers.Principal components analysis(PCA)was conducted to select the quantitative markers of the rhizomes of A.officinarum samples from different origins.The constituents were confirmed by(+)electrospray ionization LC-MS.12 constituents were selected as common peaks and 10 of them were confirmed by(+)electrospray ionization LC-MS.Six bioactive constituents including DPHA,galangin flavanone,galangin,galangin 3-methylether,DPHB and DPHC were simultaneous determination by using the HPLC-DAD analysis.The developed method was able to determine the bioactive components with excellent resolution,precision and recovery.The results indicated that chromatographic fingerprint combination with multi-components determination method is suitable for quality assessment of the rhizomes of A.officinarum.
