摘要
为了优化顶空固相微萃取(HS-SPME)和气相色谱-质谱(GC-MS)联用测定天然牧草中挥发性成分的萃取条件,试验以色谱峰总峰面积为考察指标,在单因素试验的基础上,运用Box-Behnken响应曲面法设计萃取温度、萃取时间、解析时间和样品量4因素3水平的试验模型,建立回归方程,优化筛选萃取条件。结果表明:模拟得到的最佳萃取条件为萃取温度69.60℃、萃取时间58.39 min、解析时间2.83 min、样品量2.49 g,预测色谱峰总峰面积为9.958×10^9。为了提高萃取条件的可行性,将萃取条件修正为萃取温度70℃、萃取时间60 min、解析时间3 min、样品量2.5 g,验证色谱峰总峰面积为9.842×10^9,与模型预测值较接近。说明响应曲面法优化HS-SPME-GC-MS测定天然牧草中挥发性成分的萃取条件效果好,预测值可靠。
In ordertooptimize the extraction conditions of head space solid phase microextraction(HS-SPME)and gas chromatography-mass spectrometry(GC-MS)for the determination of volatile components in natural forage,the total peak area of the chromatographic peaks was usedas the index of investigation.a three-level model with four factors including extraction temperature,extraction time,resolution time and sample sizewas designed by usingBox-Behnken response surface methodOn the basis of single factor test,and the regression equation was established and extraction conditions were optimized.The results showed that the optimal extraction temperature was 69.60°C,the optimum extraction timewas 58.39 min,the optimumanalysis time was2.83 minand the optimumsample volume was 2.49 g.The total peak area of the predicted peak was 9.958×10^9.In order to improve the feasibility of the extraction conditions,the extraction conditions were corrected as follows:extraction temperaturewas 70°C,extraction time was 60 min,analysis time was 3 min,sample amount was 2.5 g,and the total peak area of the chromatographic peak was 9.842×10^9,which was close to the predicted value of the model.The results indicated that the HS-SPME-GC-MS method optimized byresponse surface methodologywas effective and reliable in determining thevolatile constituents in natural forage.
作者
李宇宇
格根图
特日格乐
孙林
郝俊峰
降晓伟
贾玉山
LI Yuyu;Gegentu;Terigele;SUN Lin;HAJunfengJIANG Xiaowei;JIA Yushan(Key Laboratory of Forage Cultivation,Processing and High Efficient Utilization/Key laboratory of Grassland Resourcesof Ministry of Kducation/College of Grassland Resources ami Environment,Inner Mongolia Agricultural University,Hohhot 010019;College of Life Sciences,Inner Mongolia Agricultural University,Hohhot 010019;Inner Mongolia Academy of Agric-ulture and Animal Husbandry Scineces,Hohhot 010019)
出处
《黑龙江畜牧兽医》
CAS
北大核心
2020年第5期93-97,100,150,151,共8页
Heilongjiang Animal Science And veterinary Medicine
基金
“十三五”重点研发计划项目“干草低损耗高品质规模化生产及产品加工技术研究与示范”(2017YFD0502103)
国家自然基金项目“典型草原牧草刈割后干燥机制与营养物质变化相关性研究”(31760710)
国家牧草产业技术体系项目(CARS-34)。
关键词
响应曲面法
顶空固相微萃取
气相色谱-质谱联用
天然牧草
挥发性成分
萃取条件
response surface methodology
headspace solid phase microextraction
gas chromatography-mass spectrometry
natural forage
volatile components
extraction conditions