Waters液质联用仪的使用与维护保养标准操作规程

WatersQuattroPremier液质联用仪的使用与维护保养标准操作规程（SOP）2004-11-09目录1．简述······················································································································11.1样品入口····························································································21.2真空系统··········································································································21.3数据系统··········································································································22．环境要求···············································································································33．仪器使用···············································································································33.1开机步骤··········································································································33.2质谱调谐窗口各项参数设定···········································································53.3创建项目·········································································································63.4质量校正··········································································································73.5调谐(Tuning)··································································································143.6信号采集·········································································································153.72695型液相色谱（InletMethod）·······························································193.8创建质谱方法································································································253.9创建样品列 表 关于同志近三年现实表现材料材料类招标技术评分表图表与交易pdf视力表打印pdf用图表说话 pdf ·································································································273.10运行样品列表（SampleList）································································303.11QuanLynx来编辑定量方法········································································393.12用QuanLynx进行批处理··········································································443.13查看QuanLynx定量结果··········································································473.14关机···············································································································524．注意事项·············································································································535．维护与保养·········································································································54-1-1.简述QuattroPremier(Figure1-1)是一台高效串联四极杆质谱仪，用于常规LC/MS/MS 分析 定性数据统计分析pdf销售业绩分析模板建筑结构震害分析销售进度分析表京东商城竞争战略分析 。Figure1-1QuattroPremierMassSpectrometer样品的离子化发生在处于大气压状态下的离子源中。离子通过取样锥孔进入真空系统，然后穿过源travelling-wave（T-WaveTM）进入第一级四极杆，在此按照质/荷比(m/z)过滤(Figure1-2)。按照质量数分开的离子进入T-Wave碰撞室，进一步发生碰撞诱导裂解（CID）或者直接进入第二级四极杆。碎片离子通过第二级四极杆进行质量分析。离子最后经过倍增电极，phosphor和光电倍增器 检测 工程第三方检测合同工程防雷检测合同植筋拉拔检测方案传感器技术课后答案检测机构通用要求培训 系统检测。输出信号被放大，数字化后传给信号系统。-1-Figure1-2QuattroPremierSchematic1.1样品入口该仪器可以与下列两种进样方式组合：a.HPLC系统，可以提供LC流出组分的分子量信息，进行目标分析和定量。b.注射泵，分析宝贵的，低浓度的样品。HPLC系统或注射泵将样品输入ZsprayTM离子源中。通过改变探头来改变离子化模式。探头上的识别pins可以鉴别系统的离子化模式。1.2真空系统由外置的初级抽气泵和内设的涡轮分子泵提供真空系统。涡轮分子泵抽分析器和T-Wave离子传输区域的真空。初级抽气泵可以是旋转式泵或无油螺旋式泵。系统通过一个Pirani真空计监测涡轮分子泵的转速和真空度。如果真空度不够，Pirani真空计作为开关将中断仪器操作。真空隔断阀可以在不破坏真空的情况下进行离子源的日常维护。1.3数据系统包括embeddedPC，工作站和MassLynx软件。MassLynx可以控制整个系统，-2-包括设置和运行HPLC系统，仪器调谐，采集数据和数据处理。embeddedPC和工作站之间的通讯由网线连接。1.环境要求2.1仪器室要保持整洁、干净、无尘；配套设施布局合理。2.2仪器室温度应相对稳定，一般应控制在20-25℃，保持恒温；相对湿度最好为50-70%，室内应备有温度计和毛发湿度计，一般采用空调和吸湿机调节温度和湿度。2.3仪器室电源要求相对稳定，电压变化要小，最好配备不间断稳压电源，防止意外停电。2.仪器使用3.1开机步骤3.1.1分别打开质谱、液相色谱和电脑电源，此时质谱内置的CPU会通过网线与电脑主机建立通讯联系，这个时间大约需要1至2分钟。3.1.2待液相色谱通过自检，进入Idle状态，依照液相色谱操作程序，依次进行操作。a.DegasserOn(打开脱气机)。b.WetPrime(湿灌注)。c.PurgeInjector。d.平衡色谱柱。3.1.3双击桌面上的MassLynx4.0图标进入质谱软件。此时，如果进入软件时出现提示：“Theembeddedsystemisnotresponding,Thesystemwillruninstandalonemode”，则说明质谱内置的CPU（EPC）与电脑主机的通讯联系还未建-3-立，请稍等后再进入软件，如果打开软件仅为处理数据则没有关系（质谱主机电源未开时进入软件也会有同样提示）。3.1.4点击质谱调谐图标（MSTune）进入质谱调谐窗口。Figure3-1InitialTunePage3.1.5选择菜单“Options>Pump”，这时机械泵将开始工作，同时分子涡轮泵会开始抽真空。等达到真空要求后，仪器前面板右上角的状态灯“Vacuum”将变绿。3.1.6点击真空状态图标，检查真空规的状态，确认真空达到要求。2.1.7确认氮气气源输出已经打开，输出压力为90psi。3.1.8设置源温度（SourceTemp）到目标温度。-4-3.2质谱调谐窗口各项参数设定3.2.1电喷雾电离源（ESI）3.2.1.1在质谱调谐窗口选择要使用的离子模式，IonMode>Electrospray+。3.2.1.2点击进入Source界面，设定Source界面里各项参数。Capillary(KV)加在ESI源内毛细管上的高压，正离子模式一般是在2.5-3.75KV之间优化，负离子模式一般是在2.0-3.0KV之间优化。在负离子模式时，如果毛细管电压设置过高容易引起放电现象。Cone(V)样品锥孔电压，一般在10-100V之间优化，通常来说，分子量小的样品选择的锥孔电压要相对小，当提高锥孔电压时，可能得到的碎片信息会多一些。Extractor(V)二级锥孔电压，一般在0－5V之间优化。RFLen(V)六级杆透镜电压，一般在0－0.5V之间优化。SourceTemp源温度，一般在80℃－120℃之间优化，一般来讲，设定与流动相流速大小有关，如果用注射泵直接进样，流速在5－40Ul/min时，设为80℃，当液相色谱流速在100－300Ul/min时，设定为120℃。DesolvationTemp脱溶剂气温度，一般在120℃－300℃之间优化，与流动相流速大小，流动相含水比例高低，是否容易气化相关，用注射泵直接进样，流速在5－40Ul/min时，设为120，流速在5－40Ul/min时，设为80℃，当液相色谱流速在100－300Ul/min时，设为300℃。Desolvation(L/hr)脱溶剂气流量，一般在300－1000L/Hour之间优化，与-5-流动相流速大小，流动相含水比例高低，是否容易气化相关。Cone(L/hr)锥孔气的流量，一般在0－100L/Hour之间优化。3.2.1.3点击图标，进入Analyser界面，设定Analyser界面里的各项参数。LMResolution低质量数分辨率，典型值15.0。HMResolution高质量数分辨率，典型值15.0。IonEnergy离子能量，一般在0－1之间优化。Multiplier光电倍增管电压，典型值650V。3.2.2大气压化学电离源（APCI）3.2.2.1在质谱调谐窗口选择要使用的离子模式，IonMode>APCI+。3.2.2.2进入Source界面，设定Source界面里各项参数。Corona高压放电针电流，正离子模式一般在0－10之间优化，负离子模式一般在0－5之间优化。SourceTemp源温度，一般在120℃－150℃之间优化。APCIProbeTempAPCI加热器温度，一般在300℃－600℃之间优化。3.3创建项目（Project）为了便于进行数据管理，可以创建不同的项目（Project），项目的后缀为.pro，每个项目都有对应的子目录进行相应文件的管理。3.3.1从主菜单中选择“File>ProjectWizard”，会引导你去创建一个新的项目。3.3.2输入项目（project）名称及描述，点击“Next