1、岛津LC20AD液相色谱仪操作规程岛津LC-20AD液相色谱仪操作规程岛津LC-20AD型液相色谱仪操作规程 1(目的 规范岛津LC-20AD型高效液相色谱仪的使用。 2(范围 适用于岛津LC-20AD型高效液相色谱仪的使用。 3(职责 质检员对本规程的实施负责。 4(规程 4.1 系统组成:本系统由2个LC-20AD溶剂输送泵(分主/A泵和副/B泵)、SIL-20A自动进样阀、SPD-20A紫外-可见检测器、CTO-20A柱箱、LCsolution色谱数据工作站和IBM台式电脑等组成。 4.2 准备 4.2.1 准备所需的流动相，用合适的0.45m滤膜过滤，超声脱气20min。 4.2.2
2、根据待检样品的需要更换合适的洗脱柱(注意方向)和定量环。 4.2.3 配制样品和标准溶液(也可在平衡系统时配制)，用合适的0.45m滤膜过滤。 4.2.4 检查仪器各部件的电源线、数据线和输液管道是否连接正常。 4.3 开机 4.3.1 接通电源，依次开启不间断电源、B泵、自动进样器、检测器、柱温箱、A泵 4.3.2 待泵和检测器自检结束后，打开打开色谱工作站，点击按钮“1”，输入用户名:ADMIN。 4.3.3 当SPD-20A发出蜂鸣声后，说明已建立与计算机之间的连接，LC窗口打开。 4.4 参数设定 4.4.1 设置新的分析参数时，请从通过键盘在LC窗口 的“Instrument Par
3、ameters View”中输入参数(即A、B泵的流速，波长，柱温;柱在线时流速一般不超过1ml/min) 4.4.2 选择 File Save Method File As ，输入方法名称后保存。 4.4.3 点击“Download”键，将保存好的方法下载 4.5 更换流动相并排气泡 4.5.1 将A/B管路的吸滤器放入装有准备好的流动相的储液瓶中; 4.5.2 逆时针转动A/B泵的排液阀360? 4.5.3 按A/B泵的purge键，pump指示灯亮，1min再次按A/B泵的purge键 4.5.4 顺时针转动A/B泵的排液阀,关闭排液阀 4.5.5 如管路中仍有气泡，则重复以上操作直至气
4、泡排尽 4.6 平衡系统 4.6.1 更换流动相并排气泡后，在工作站中输入实验信息并设定各项方法参数 4.6.2 等度洗脱方式 4.6.2.1 点击“Instrument on/off ”按钮， A、B泵将同时启动，pump指示灯亮。用检验方法规定的流动相冲洗系统，一般最少需6倍柱体积的流动相。 4.6.2.2 检查各管路连接处是否漏液，如漏液应予以排除。 4.6.2.3 观察泵控制屏幕上的压力值，压力波动应不超过1MPa。如超过则可初步判断为柱前管路仍有气泡，应重新排气泡。 4.6.2.4 观察基线变化。如果冲洗至基线漂移0.01mV/min，噪声为0.001mV时，可认为系统已达到平衡状态
5、，可以进样。 4.6.3 梯度洗脱方式 4.6.3.1 以检验方法规定的梯度初始条件，按4.6.2项下方法平衡系统。 4.6.3.2 在进样前运行12次空白梯度。 4.7 进样 4.7.1 进样前按软件中零点校正 按钮校正基线零点 4.7.2 点击“Single start ”按钮，设置好保存路径并输入试样位置，系统开始自动进样 4.7.3 样品采集完毕后，点击“Stop”按钮，接着就会出现一条消息，询问您是否“Abort the current run”, 单击Yes，当前的数据采集就会终止。 4.8 清洗系统和关机 4.8.1 数据采集完毕后，关闭泵，待压力降为0后，将工作流动相换水相，设
6、定流动相比例，冲洗色谱柱 4.8.2 清洗柱 4.8.2.1 C18柱先用95%的水以1ml/min冲洗40min以上，再用90%的甲醇或乙腈冲洗20min，最后用40%的水冲洗10min 4.8.2.2 Protein PAK60柱先用超纯水冲洗90min以上，再用甲醇或乙腈冲洗40min 4.8.3 清洗完成后，先关闭泵，待压力降至为“0”时，关闭各组件电源，关闭计算机 4.9 填写使用记录。 高效液相使用与维护记录 仪器型号: 日期 开机 关机 样品名称 仪器 使用人 复核人 备注 时间 时间 情况 高效液相使用与维护记录 仪器型号: 日期 开机 关机 样品名称 仪器 使用人 复核人 备
7、注 时间 时间 情况 (英文版 ) Two regulations promulgated for implementation is in the party in power for a long time and the rule of law conditions, the implementation of comprehensive strictly strategic plan, implementation in accordance with the rules and discipline to manage the party, strengthen inner-part
8、y supervision of major initiatives. The two regulations supporting each other, the adhere to a positive advocate, focusing on morality is of Party members and Party leading cadres can see, enough to get a high standard; around the party discipline, disciplinary ruler requirements, listed as negative
9、 list, focusing on vertical gauge, draw the party organizations and Party members do not touch the bottom line . Here, the main from four square face two party rules of interpretation: the first part introduces two party Revised regulations the necessity and the revision process; the second part is
10、the interpretation of the two fundamental principles of the revision of laws and regulations in the party; the third part introduces two party regulations modified the main changes and needs to grasp several key problems; the fourth part on how to grasp the implementation of the two regulations of t
11、he party. and revised the necessity and revised history of the CPC Central Committee the amendment to the Chinese Communist Party members and leading cadres honest politics several guidelines and column 1 by 2015 to strengthen party laws and regulations focus. Two party regulations revision work las
12、ted a Years, pooling the wisdom of the whole party, ideological consensus, draw historical experience, respect for the wisdom of our predecessors, which reflects the unity of inheritance and innovation; follow the correct direction, grasp the limited goals, adhere to the partys leadership, to solve
13、the masses of the people reflect a focus on the problem. The new revision of the and , reflects the partys 18 and the eighth session of the third, the spirit of the fourth plenary session, reflecting the experience of studying and implementing the General Secretary Xi Jinping series of important spe
14、ech, reflects the partys eighteen years comprehensive strictly practice. (a) revised two regulations of the party need of in based on revised, the promulgation and implementation of January 2010, to strengthen the construction of the contingent of leading cadres play an important role. But with the
15、party to manage the party strictly administering the deepening, has not been able to fully meet the actual needs. Content is too complicated, eight prohibition, 52 are not allowed to hard to remember, and also difficult to put into practice; the second is concisely positive advocated by the lack of
16、prohibited provisions excessive, no autonomy requirements; the third is banned terms and discipline law, both with the party discipline, disciplinary regulations repeat and Criminal law and other laws and regulations repeat; the fourth is to clean the theme is not prominent, not for the existing pro
17、blems, and is narrow, only needle of county-level leading cadres above. is in 1997 based on revision, in December 2003 the promulgation and implementation, to strengthen the construction of the party play very important role. Along with the development of the situation, which many provisions have be
18、en unable to fully meet the comprehensive strictly administering the practice needs. One is Ji law, more than half of the provisions and criminal law and other countries laws and regulations Repetition; two is the political discipline regulations is not prominent, not specific, for violation of the
19、party constitution, damage the authority of Party Constitution of misconduct lack necessary and serious responsibility to pursue; third is the main discipline for the leading cadres, does not cover all Party members. Based on the above situation, need to and the two is likely to be more relevant reg
20、ulations first amendment. By revising, really put the authority of Party discipline, the seriousness in the party tree and call up the majority of Party members and cadres of the party constitution of party compasses party consciousness. (II) two party regulations revision process the Central Commit
21、tee of the Communist Party of China attaches great importance to two regulations revision . Xi Jinping, general books recorded in the Fifth Plenary Session of the eighth session of the Central Commission for Discipline Inspection, on the revised regulations made clear instructions. According to the
22、central deployment, the Central Commission for Discipline Inspection from 2014 under six months begin study two regulations revision. The Standing Committee of the Central Commission for Discipline Inspection 4 review revised. Comrade Wang Qishan 14 times held a special meeting to study two regulati
23、ons revision, amendment clarifies the direction, major issues of principle, path and target, respectively held a forum will listen to part of the province (area) secretary of the Party committee, Secretary of the Discipline Inspection Commission, part of the central ministries and state organs Depar
24、tment The first party committee is mainly responsible for people, views of experts and scholars and grassroots party organizations and Party members. Approved by the Central Committee of the Communist Party of China, on 7 September 2015, the general office of the Central Committee of the Party issue
25、d a notice to solicit the provinces (autonomous regions, municipalities) Party, the central ministries and commissions, state ministries and commissions of the Party (party), the General Political Department of the military, every 3 people organization of Party of two regulations revision opinion. C
26、entral Commission for Discipline Inspection of extensive solicitation of opinions, careful study, attracting, formed a revised sent reviewers. In October 8 and October 12, Central Committee Political Bureau Standing Committee and the Political Bureau of the Central Committee After consideration of t
27、he two regulations revised draft. On October 18, the Central Committee of the Communist Party of China formally issued two regulations. Can say, two laws amendment concentrated the wisdom of the whole party, embodies the party. Second, and revision of the basic principles of two party regulations re
28、vision work and implement the partys eighteen, ten eight plenary, the spirit of the Fourth Plenary Session of the Eleventh Central Committee and General Secretary Xi Jinping important instructions on the revised and , highlighting the ruling party characteristics, serious discipline, the discipline
29、quite in front of the law, based on the current, a long-term, advance as a whole, with Bu Xiuding independent and . Main principle is: first, adhere to the party constitution to follow. The constitution about discipline and self-discipline required specific, awaken the party constitution of party co
30、mpasses party consciousness, maintaining the authority of the constitution. General Secretary Xi Jinping pointed out that no rules, no side round. Party constitution is the fundamental law, the party must follow the general rules. In early 2015 held the eighth session of the Central Commission for D
31、iscipline Inspection Fifth Plenary Session of the 16th Central Committee, Xi Jinping again pointed out that constitution is the party must follow the general rules, but also the general rules. the revision of the and is Method in adhere to the regulations established for the purpose of combining rule of virtue is to adhere to the party constitution as a fundamental to follow, th
