色谱柱和色谱系统的故障检修(生产管理 质量管理 成本管理 品质管理).ppt

* Column Aging/Equilibration Causes Retention/Selectivity Changes柱老化／平衡不够引起保留时间／选择性改变 Column 1 - Initial 1 号柱 开始时 Column 1 - Next Day 1 号柱 第二天 Column 1 - After Cleaning with 1% H3PO4 1 号柱用 1% H3PO4 清洗 The primary analyte was sensitive to mobile phase aging of the column. 最初的分析对流动相老化柱子是灵敏的 The peak shape was a secondary issue resolved by flushing the column. 冲洗柱子第二要解决的问题是峰形 Retention and peak shape were as expected after cleaning. 清洗后保留时间和峰形都达到了预期效果 * 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 * 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 * 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 * 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