简介:建立鸡肉中糖皮质激素多残留的液相色谱-串联质谱分析方法。样品经乙酸乙酯提取,正己烷净化,10%乙腈水定容后供高效液相色谱-串联质谱仪(LC-MS/MS)分析,采用C18色谱柱分离,电喷雾离子化负离子方式(ESI-)及多反应监测模式(MRM)进行测定,外标法定量。研究了仪器条件、提取溶剂、净化溶剂等条件对七种目标物分离状况的影响。在优化条件下,该方法在鸡肉样品中泼尼松的的线性范围为0.5-20μg/L,泼尼松龙、甲基泼尼松、地塞米松、氢化可的松、倍氯米松、氢化可的松乙酸盐的浓度范围为0.1-20μg/L,在加标水平1.0-10μg/kg范围内,回收率为83%-104.2%;相对标准偏差为0.92%-4.89%。
简介:Weprovidethefirstdemonstrationofpureredemissioninthevisiblelightregionviathree-photonexcitationinmonodisperseNa_3ZrF_7:Ernanoparticles(NPs)byusingalaseroperatinginthetelecommunicationband.NPsof~22nmindiameteraresynthesizedat260°Cbythethermaldecompositionmethod.TheexperimentalresultsrevealthattheNa_3ZrF_7:ErNPsexhibitpureredemissioninthevisibleregionunder1480nmlaserexcitation,andtheemissionintensityissignificantlyinfluencedbytheEr~(3+)ionconcentration.Thedecaytimesofthe~4S_(3∕2)→~4F_(15∕2)and~4F_(9∕2)→~4F_(15∕2)transitionsoftheEr~(3+)ionsat540and655nm,respectively,arereducedbyincreasingtheEr~(3+)ionconcentrationintheNa_3ZrF_7:ErNPs.Thesuppressedemissionintensityresultfromthedefect-relatedquenchingeffect:whentrivalentEr~(3+)ionsreplactetravalentZr~(4+)ions,extraNationsandFvacanciesareformedtore-balancethechargeintheNa_3ZrF_7matrix.TheemissioncoloroftheNa_3ZrF_7:ErNPsisrelatedtothecrossrelaxationbetweenEr~(3+)ions.Theseresultsprovideanimportantsteptowardmoreeffectivebiologicalimagingandphotodynamictherapybyminimizingthescatteringoftheexcitationlightandincreasingthepenetrationdepth.