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作 者:张倩[1,2] 贝峰[3] 孙欣[2] 王明林[2] 辛力[1]
机构地区:[1]山东省果树研究所,山东泰安271000 [2]山东农业大学食品科学与工程学院,山东泰安271000 [3]泰安出入境检验检疫局,山东泰安271000
出 处:《果树学报》2017年第10期1294-1300,共7页Journal of Fruit Science
基 金:山东省现代农业产业技术体系水果创新团队建设(SDAIT-06-13);山东省农业重大应用技术创新项目--樱桃采后商品化处理设备研制与试验示范;泰安市科技计划重大专项(201340629)
摘 要:【目的】寻求建立甜樱桃果实中赤霉酸的定性定量检测方法,为研究赤霉素在大棚甜樱桃的使用安全性上提供方法参考。【方法】样品经乙腈提取,液-液分配法进行净化,采用高效液相色谱-串联质谱(HPLC-MS/MS)法在SRM模式下对目标物质进行定性和定量检测。【结果】方法的最低检出限(S/N=3)为1.21μg·kg^(-1),定量限(S/N=10)为4.03μg·kg^(-1),在5.0~100.0μg·L^(-1)内呈现良好的线性关系,相关系数r2为0.999 3,添加浓度为0.001、0.002、0.01 mg·kg^(-1)时赤霉素加标回收率分别为89.69%,91.84%和95.37%(n=6),相对标准偏差分别为7.46%,6.21%和4.85%,方法的不确定度为0.13μg·kg^(-1),5份大棚樱桃样品中GA_3含量在21.3~71.1μg·kg^(-1)。【结论】本方法简单快速,灵敏度高,定量准确,可用于樱桃果实中的赤霉素残留量测定。[Objective] Some varieties of sweet cherry are not self-fertile, so pollinizer varieties are need- ed. Inappropriate temperature and rainfall during bloom affect pollination and fertilization, resulting in flower and fruit drop. Plant growth regulator (mainly GA) treatment during full bloom can significantly increase fruit set in cherry. In this study, we developed a method for the determination of gibberellic acid in sweet cherry fruit using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/ MS), which provides support for studying roles of GA in fruit set. [Methods] 5.00 g cherry sample was ac- curately weighed and put into a 50 mL polypropylene centrifuge tube, to which. 25 mL acetonitrile and 2.0 g sodium chloride were added. After capped, the sample was vortex mixed for 1 min, and the suspension was centrifuged for 10 min at 4 000 r· min-1. The supernatant acetonitrile layer was transferred into a flask. The extraction procedure was repeated twice and the supernatant acetonitrile layers from the centrifuges were combined, which was then evaporated to dryness in a rotary evaporator at 45 ℃. The residue was dissolved in 10 mL sulphuric acid-water (pH 2.5) solution and added with 20 mL ethyl acetate and transferred into a 50 mL centrifuge tube. The centrifuge tube was then vortex mixed for 1 min before centri- fuged for 10 min at 4 000 r· min-1. The ethyl acetate layer was transferred into a flask. The extraction was repeated twice and the ethyl acetate fractions were combined. Then 10 mL phosphate buffer solution (pH 7.5) was added into extracted ethyl acetate extract and shaken vigorously for 30 s before vortex mixed for 1 min. The suspension was centrifuged for 10 min at 4 000 r· min-1. The phosphate buffer solution layer was transferred into a centrifuge tube. The extraction was repeated twice and the extracted phosphate buf- fer fractions were combined and adjusted to pH 2.5 using sulphuric acid-water (1:1). Then 20 mL ethyl acetate was added and vortex mix
关 键 词:甜樱桃 赤霉酸 高效液相色谱-串联质谱 定性定量检测
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