高效液相色谱法分析内生真菌草酸青霉的代谢产物黑麦酮酸A  

Determination of Secalonic Acid A from Endophytic Fungus Penicillium Oxalicum by High Performance Liquid Chromatography

作　　者：王艳红[1] 吴晓民[2] 朱艳萍[1] 杨信东[3] 李月茹[1] 

机构地区：[1]吉林农业大学农业部参茸产品质量监督检验测试中心,长春130118 [2]吉林农业大学附属医院,长春130118 [3]吉林农业大学农学院,长春130118

出　　处：《分析化学》2013年第4期575-579,共5页Chinese Journal of Analytical Chemistry

基　　金：吉林农业大学科研启动基金(No.201110)资助项目

摘　　要：建立了高效液相色谱法(HPLC)测定内生真菌草酸青霉发酵液中黑麦酮酸A的方法。采用AgilentXDB-C18色谱柱(250 mm×4.6 mm,5μm),确定了最佳色谱条件:流动相为甲醇和水(70∶30,V/V),DAD检测器,检测波长为320 nm,流速为0.8 mL/min,柱温为30℃,进样量20μL。结果表明,在0.4～22 mg/L范围内,相关系数r=0.9996。在加标水平为0.5,5.0和15.0 mg/L时,平均回收率为86.0%～106.7%;相对标准偏差RSD<6%;检出限为0.08 mg/L,具有较好的精密度和准确度。本方法已对10批实际样品进行发酵提取和分析,RSD=4.4%,可应用于内生真菌发酵优化过程中代谢产物黑麦酮酸A的定量分析。The secondary metabolite secalonic acid A from endophytic fungus has strong antitumor anti-inflammatory and antibacterial activities,which shows good development prospects for the new drugs.A method was developed for the determination of secalonic acid A in the broth of endophytic fungus Penicillium oxalicum by high performance liquid chromatography.Agilent XDB-C18（250 mm × 4.6 mm,5 μm） and DAD detector were used for the determination of secalonic acid A under the conditions as follows： methanol and water（70 ∶ 30,V/V） as mobile phase with a flow rate of 0.8 mL/min,320 nm of detection wavelength,30 ℃ of column temperature,and 20 μL of sample volume.The linearity,the detection limit,the precision and recovery were analysed.The results showed a good linear relationships in the range of 0.4-22 mg/L with a correlation coefficient of 0.9996.The mean recoveries were in the range of 86.0%-106.7% at three spiked levels of 0.5,5.0 and 15.0 mg/L,and the relative standard deviations（RSDs） were less than 6%.The limit of detection was 0.08 mg/L.The proposed method had successfully used for the analysis of ten batches of real samples with 4.4% of RSD,which showed that the method can be applied in the analysis of secondary metabolity secalonic acid A in the fermentation process from endophytic fungi.

关 键 词：高效液相色谱 内生真菌 代谢产物 黑麦酮酸A 

分 类 号：TQ920.6[轻工技术与工程—发酵工程] O657.72[理学—分析化学]