Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo a...Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo and in vitro. In this work, wheat culture was inoculated with a Fusarium graminearum PH-1 strain for DON production. The solvent system for crude extraction was acetonitrile-water（84：16, v/v）. A simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography（preparative HPLC） to purify the compound. The solvent system for the second silica gel column chromatography was methylene chloride-methanol（17：1, v/v）, which provided a good elution effect selected on thin layer chromatography（TLC）. The target compound was identified by HPLC, and the chemical structure was confirmed by mass spectrometry（MS） and ~1H and ^（13）C nuclear magnetic resonance（NMR） spectroscopy. A total of 433 mg of purified DON was obtained from 1 kg of wheat culture, with a purity of 99.01%. The study had provided an easy-operating and cost-effective method to isolate an expensive compound in a simple way.展开更多
以实验室自制1,3-二油酸甘油二酯粗品(含量76.41%)为原料,采用硅胶柱色谱法制备高纯1,3-二油酸甘油二酯。通过硅胶薄层色谱对4种混合溶剂洗脱剂进行筛选,确定硅胶柱色谱最佳洗脱剂为D(正己烷-乙酸乙酯-乙醚-乙酸的混合液)。以1,3-二油...以实验室自制1,3-二油酸甘油二酯粗品(含量76.41%)为原料,采用硅胶柱色谱法制备高纯1,3-二油酸甘油二酯。通过硅胶薄层色谱对4种混合溶剂洗脱剂进行筛选,确定硅胶柱色谱最佳洗脱剂为D(正己烷-乙酸乙酯-乙醚-乙酸的混合液)。以1,3-二油酸甘油二酯的回收率和纯度为指标,系统考察了硅胶柱色谱的洗脱流速、上样质量浓度、硅胶量对纯化效果的影响,确定最佳硅胶柱色谱纯化条件为:洗脱流速1.5 m L/min,上样质量浓度75 mg/m L(上样体积10 m L),硅胶量30 g。该条件下制得的1,3-二油酸甘油二酯样品纯度达98.03%,回收率为69.90%。展开更多
采用硅胶柱层析法对菌体内醇溶性红曲黄色素进行分离、纯化,并对纯化后的红曲黄色素结构及纯度进行液相质谱鉴定表征,得到柱层析最佳洗脱条件:洗脱剂配比正己烷∶乙酸乙酯(v/v)=1∶8,上样量1.5 m L,洗脱流速50 m L/h。分离纯化所得的红...采用硅胶柱层析法对菌体内醇溶性红曲黄色素进行分离、纯化,并对纯化后的红曲黄色素结构及纯度进行液相质谱鉴定表征,得到柱层析最佳洗脱条件:洗脱剂配比正己烷∶乙酸乙酯(v/v)=1∶8,上样量1.5 m L,洗脱流速50 m L/h。分离纯化所得的红曲色素经液相质谱检测含红斑胺素、红曲素、红斑素三种色素组分,采用相对定量法对分离所得的红曲黄色素组分进行纯度表征,结果显示其纯化保存率达85%。展开更多
基金supported by the National Natural Science Foundation of China (31402268)the Natural Science Foundation of Jiangsu Province of China (BK20140691)+1 种基金Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions (PAPD), ChinaThe Introduction of International Advanced Agricultural Science and Technology Project from the Ministry of Agriculture of China (2012-Z22)
文摘Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo and in vitro. In this work, wheat culture was inoculated with a Fusarium graminearum PH-1 strain for DON production. The solvent system for crude extraction was acetonitrile-water（84：16, v/v）. A simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography（preparative HPLC） to purify the compound. The solvent system for the second silica gel column chromatography was methylene chloride-methanol（17：1, v/v）, which provided a good elution effect selected on thin layer chromatography（TLC）. The target compound was identified by HPLC, and the chemical structure was confirmed by mass spectrometry（MS） and ~1H and ^（13）C nuclear magnetic resonance（NMR） spectroscopy. A total of 433 mg of purified DON was obtained from 1 kg of wheat culture, with a purity of 99.01%. The study had provided an easy-operating and cost-effective method to isolate an expensive compound in a simple way.
文摘以实验室自制1,3-二油酸甘油二酯粗品(含量76.41%)为原料,采用硅胶柱色谱法制备高纯1,3-二油酸甘油二酯。通过硅胶薄层色谱对4种混合溶剂洗脱剂进行筛选,确定硅胶柱色谱最佳洗脱剂为D(正己烷-乙酸乙酯-乙醚-乙酸的混合液)。以1,3-二油酸甘油二酯的回收率和纯度为指标,系统考察了硅胶柱色谱的洗脱流速、上样质量浓度、硅胶量对纯化效果的影响,确定最佳硅胶柱色谱纯化条件为:洗脱流速1.5 m L/min,上样质量浓度75 mg/m L(上样体积10 m L),硅胶量30 g。该条件下制得的1,3-二油酸甘油二酯样品纯度达98.03%,回收率为69.90%。
文摘采用硅胶柱层析法对菌体内醇溶性红曲黄色素进行分离、纯化,并对纯化后的红曲黄色素结构及纯度进行液相质谱鉴定表征,得到柱层析最佳洗脱条件:洗脱剂配比正己烷∶乙酸乙酯(v/v)=1∶8,上样量1.5 m L,洗脱流速50 m L/h。分离纯化所得的红曲色素经液相质谱检测含红斑胺素、红曲素、红斑素三种色素组分,采用相对定量法对分离所得的红曲黄色素组分进行纯度表征,结果显示其纯化保存率达85%。
