LCMS-岛津工程师培训

岛津国际贸易（上海）有限公司分析中心岛津LCMS-2010EV培训班2ShimadzuInternationalTrading(Shanghai)Co.Limited主要内容1.LC/MS简介2.LC结构特点3.LC/MS离子化接口4.MS质量分析器5.MS的结构特点6.LC分析条件至LC/MS分析条件的转化7.LC/MS应用举例3ShimadzuInternationalTrading(Shanghai)Co.Limited1.LC/MS简介ShimadzuLC-10Avp/LCMS-2010AsystemShimadzuLC-20A/LCMS-2010EVsystem4ShimadzuInternationalTrading(Shanghai)Co.LimitedLCMS-2010A系统LCMS-2010ALC-10AvpLCMS-2010LCMSsolution5ShimadzuInternationalTrading(Shanghai)Co.LimitedLCMS-2010LCMSsolutionLC-20A岛津新型LCMS系统LCMS-2010EV6ShimadzuInternationalTrading(Shanghai)Co.Limited6何种化合物可用LC/MS分析?取决于化合物的离子化效率；化合物分子自身的极性，结构及其所含的功能基团等因素均会影响离子化情况；多数具有一定极性的有机化合物可以通过ESI或APCI的方式离子化，如:药物及其代谢产物天然产物(生物碱,配糖物、苷glycosides,taxanes,毒素,糖类,脂类,维生素等等)蛋白质，多肽；杀虫剂，除草剂表面活性剂和染料7ShimadzuInternationalTrading(Shanghai)Co.LimitedLC/MS的优势强大的定性和选择性能力多组份样品的准确定性；未充分分离组份峰的鉴别；消除杂质干扰；可作为便捷的定性分析用于合成和衍生反应的研究；作NMR预分析的质谱鉴定；广泛适用于难挥发性化合物的分析扩展了大气压离子化API的多种应用8ShimadzuInternationalTrading(Shanghai)Co.Limited对液相色谱分离组份进行强有力的定性确证M/ZM/ZM/Z[TIC色谱图][质谱图]9ShimadzuInternationalTrading(Shanghai)Co.Limited基本名词解释TICTotalIonChromatogram总离子流色谱图MCMassChromatogram质量色谱图Achromatogramthatisobtainedbyplottingdataatarbitrarym/zvaluesamongthemassspectrumdatarepeatedlycollectedatgivenintervalsMICMixedIonChromatogram混合离子流色谱图CDLCurveddesolvationline曲线脱溶剂管SIMSelectedIonMonitoring选择性离子检测方式SCAN10ShimadzuInternationalTrading(Shanghai)Co.Limited同位素丰度比AA+1A+2C1001.11H1000.015N1000.37O1000.040.20F100Si1005.063.36P100S1000.794.43Cl10031.99Br10097.28I10011ShimadzuInternationalTrading(Shanghai)Co.Limited多组份样品的准确鉴定黄曲霉毒素的分析5.06.07.08.09.010.011.012.013.014.015.0min0e3250e3500e3750e31000e31250e3Int.MIC331.20287.20329.20285.20315.20313.20AFG2AFG1AFB2AFB1OOOOOOCH3OOOOOOCH3OOOOOOCH3HOOOOOOOOCH3OOOOOOOCH3OOOOOOOCH3HOOOOOOOCH3OHOOOOOOCH3OHB2aB2B1G2aG2G1M2M1100125150175200225250275300325350375400425450475m/z0e3100e3200e3300e3400e3Int.331.2287.1269.5313.4167.2392.2241.4100125150175200225250275300325350375400425450475m/z0e3250e3500e3Int.315.1289.2133.0黄曲霉毒素G2黄曲霉毒素B2由于黄曲霉毒素有许多异构体，因此对不同异构体选择性分析非常重要。LC/MS能够准确从色谱图相应的MS谱图识别不同的异构体。MW=330MW=31412ShimadzuInternationalTrading(Shanghai)Co.Limited强大的选择性A:100D:150B:100C:150m/z=150TICm/z=100ABCD13ShimadzuInternationalTrading(Shanghai)Co.Limited未充分分离峰的鉴别椰子油的分析2.55.07.510.012.515.017.5min0e610e620e630e640e650e660e6Int.三烷基甘油用反相HPLC方式分离，洗脱次序基于同系物的炭数ECN=CN-2xDBElutionorderisbasedonequivalentcarbonnumberm/z439.5:C38DB=0m/z467.5:C40DB=1m/z495.5:C42DB=2m/z523.5:C44DB=3TIC14ShimadzuInternationalTrading(Shanghai)Co.Limited2.LC结构特点15ShimadzuInternationalTrading(Shanghai)Co.Limited液相色谱流程图输液泵进样器色谱柱柱温箱检测器溶剂MS16ShimadzuInternationalTrading(Shanghai)Co.Limited液相色谱仪器系统分类等度系统梯度系统高压梯度系统2台输液泵低压梯度系统1台输液泵＋梯度比例阀＋在线脱气机17ShimadzuInternationalTrading(Shanghai)Co.Limited混合器低压梯度比例阀高压梯度低压梯度脱气机高压/低压梯度系统18ShimadzuInternationalTrading(Shanghai)Co.Limited高压梯度系统梯度准确度好系统复杂(需两台或三台泵)低压梯度系统系统简单需在线脱气机梯度延迟体积比高压梯度系统大高压/低压梯度系统19ShimadzuInternationalTrading(Shanghai)Co.Limited液相色谱仪器主要部件吸滤头脱气机输液泵混合器进样器色谱柱柱温箱检测器20ShimadzuInternationalTrading(Shanghai)Co.Limited吸滤头过滤去除流动相中不溶性颗粒吸滤头部件号：228-45707-91吸滤头部件号：228-21984-0121ShimadzuInternationalTrading(Shanghai)Co.Limited输液泵LC-20AT串联式柱塞往复泵耐用性好LC-20AD并联式柱塞往复泵脉动小，适合于半微量LC和LC-MSLC-20AB二联泵体积小，单独构成二元高压梯度系统22ShimadzuInternationalTrading(Shanghai)Co.Limited柱塞往复泵单向阀马达和凸轮柱塞杆柱塞杆密封圈泵头10-100uL23ShimadzuInternationalTrading(Shanghai)Co.LimitedLC-20AT24ShimadzuInternationalTrading(Shanghai)Co.LimitedLC-20AD25ShimadzuInternationalTrading(Shanghai)Co.LimitedLC-20AB26ShimadzuInternationalTrading(Shanghai)Co.Limited混合器常规混合器具有优良梯度性能的梯度混合器。具有3个阶段的混合体积，0.5、1.7、2.6ml。可以用于高压、低压或半微量梯度分析。半微量混合器具有优良梯度性能的半微量梯度混合器。混合体积为100ul。27ShimadzuInternationalTrading(Shanghai)Co.Limited进样器手动进样器7725i常规手动进样器(20ul)8125i半微量手动进样器(5ul)自动进样器SIL-20A/20AC自动进样器(100ul)28ShimadzuInternationalTrading(Shanghai)Co.Limited自动进样器SIL-20A/20AC概要SpecificationsSIL-20A（228-45006-XX）SIL-20AC（228-45007-XX）InjectionsystemTotalvolumeinjection,VariableinjectionvolumeInjectionvolumesettingrange0.1μLto100μL(standard),1μLto2,000μL(optional)Numberofsampleprocessed175(1mLvials)+10(1.5mLvials)105(1.5mLvials)+10(1.5mLvials)50(4mLvials)+10(1.5mLvials)2(96-well,384-wellMTP/DWP)+10(1.5mLvials)175(1mLvials)+10(1.5mLvials)70(1.5mLvials)+10(1.5mLvials)50(4mLvials)+10(1.5mLvials)2(96-well,384-wellMTP/DWP)+10(1.5mLvials)Injectionaccuracy±1%Injectionprecision0.3%RSDorless(10μLinjection)Samplecarryover0.005%orless(Naphthalene/Chlorhexidine)SamplecoolingNone4ºCto40ºCSIL-20ACVialrackControlvialrackNeedlemotorMeteringpumpPeltierdeviceInjectionport29ShimadzuInternationalTrading(Shanghai)Co.Limited色谱柱Shim-packVP-ODS150×4.6mm5umShim-packVP-ODS150×2.0mm5um30ShimadzuInternationalTrading(Shanghai)Co.Limited柱温箱模块式柱温箱CTO-10ASvp强制空气循环式柱温箱CTO-20A/20AC31ShimadzuInternationalTrading(Shanghai)Co.LimitedCTO-20A/20AC的概要SpecificationsCTO-20A（228-45009-XX）CTO-20AC（228-45010-XX）OventypeForcedaircirculationTemperaturecontrolrangeAmbient+10ºCto85ºCAmbient-10ºCto85ºCTemperatureprecision0.1ºCorlessTemperatureprogrammingYes(linearandstep)CTO-20ACCMDMixerValvesInjecto