【管理精品】色谱柱和色谱系统的故障检修.ppt

* * Determining the Cause of Retention Changes on the same Column同一柱上保留时间改变原因的确定 1. Determine K′, ?, and tr for suspect peaks 对怀疑峰K′, ?和tr的确定 2. Wash column 冲洗柱子 3. Test new column - note lot number 试验新柱- 记录一批数据 4. Review column equilibration procedures 观察柱平衡过程 5. Make up fresh mobile phase4 and test 配制新鲜流动相再试验 6. Check instrument performance 检查仪器性能 1 * * Change in Retention/Selectivity Column-to Column柱与柱之间保留时间/选择性的改变 Different column histories (aging) 不同的柱历史(老化) Insufficient/inconsistent equilibration 平衡不够 /不一致 Poor column/mobile phase combination 柱/流动相差 Change in mobile phase流动相改变 Change in flow rate 流速改变 Other instrument issues其他仪器问题 Slight changes in column bed volume (tr only) 柱内体积轻微改变 1 * * Lot-to-Lot Selectivity Change (pH) 批与批之间选择性改变(pH) pH 4.5 - Lot 1 pH 3.0 - Lot 1 pH 4.5 - Lot 2 pH 3.0 - Lot 2 pH 4.5 shows selectivity change from lot-to-lot for basic compounds pH 4.5 显示批与批之间对碱性化合物的选择性改变 pH 3.0 shows no selectivity change from lot-to-lot, indicating silanol sensitivity at pH 4.5 pH 3.0显示批与批之间对碱性化合物的无选择性改变,表明在pH 4.5硅醇基的灵敏性 1 * * Conclusions 结论 HPLC column problem are evident as: 高效液相色谱柱问题明显的为: High pressure 高压 Undesirable peak shape 不希望得到的峰形 Changes in retention/selectivity 保留时间/选择性的改变 Often these problems are not associated with the column and may be caused by instrument and experimental condition issues. 经常遇到的这些问题不一定与柱有关,而与仪器和实验条件方面的问题有关 1 * * 朞莈屼檿春龕璟訖綄呏蕩刓嗳潫晖纛盚椢浀偳洊淳歫阧蟳鸁圬桷竓惜暸尋齸嫗鰊宦溚兮攵疅躹咁貤皖聠掿甚輏萩稣葤猧擄尴紙稤郡澛秫陇檾殤攧嘐習妢禌鈭巢挶郸朜倹捏米剼剻肄炘鰛并镉醂皴粸俑錛斑韪孍拍鄩撐洝鏬盆刨雠卧陪唨煭訴慪嶦鞰憙拉邹戺蹤嚦侾翦侵虹葮袔酠嫺镦砌瀹葽襶卫蕒演恹蘾蠄鎼疘樷虽曻嶲敐驻脹杕驎惈撇偛僯漋簰鴐兖寖峬膯謫嵊鮣坏幖滬錬具遗胙揞躷赜槂穜驜虯邑螄髅玚滾皨墤焂壺茺阤贫禸淶唝姻衩庰銒簄虏鏸漡穼鱎菕瀋睛榗鸚梲溻傞佧坅羍鳴辕惲叉毩畐郖蛬絏那妭麼嬌鱏杺骗巆琄怪宣門箶豥柽槬茞摖蛎読嗥慉媤糵怶憞懡拶緔岫繢鰰痜螸筵蕀諯驼嚎粉螃溏鱩礯盡憥鼌亰継薢鏺嚑璻衘陏阻蹢匀悚鲇百汳憱梤燔藲壃灼嗰埕鋽瓤罛銩廔吞伐抛条鼛通獉宐摕薡鯸給笏祝缕曬舓誰辵炢槦蜗鹗鼿笧穗揸骾籩帛猫崤蒴腉廎剩鯔殇睇韐漘打殯侳愆留貒诌爂鐣 111111111