HPLC Troubleshooting & Its Data Integrity Assessment
HPLC (High Performance Liquid Chromatography) is a chromatographic technique used to separate a mixture of compounds between Mobile phase and stationary phase. The technique is widely used in industrial area and sometimes troubleshooting as mentioned below need to be done for the well functioning of the technique.
Baseline Troubleshooting: Several factors can contribute to improper baseline which needs to be checked as defined below.
|Gas in the mobile phase||Need to Degas the Mobile phase|
|Leakages||Need to fix the leakages|
|Air in the pump||Prime the pump|
|Aged Detector lamp||Replace the detector lamp (you can define light intensity criteria to replace the lamp)|
|Gas in the detector||To be removed by back-pressure of the system.|
|Detector not cleaned||Can be cleaned by 6N nitric acid|
|Valves not cleaned||Clean the valves|
|Plunger not working||Replace the plunger|
|Variation in back||Filter the solvent & samples|
Poor/Distorted Peak or No Peak:
|Dead/Aged Column||Replace the column|
|Aged Detector lamp||Replace the lamp|
|Connections not proper||Check the connections|
|Mobile phase not accurate||Check the mobile phase and change|
|In-correct Column||Check & replace|
|Leakages||Need to fix|
|Air bubbles||Degas the Mobile phase and flush the system|
|Incorrect/ contaminated guard column||Replace the Guard column|
|Dried column if not stored with end caps||Store column with end caps|
As on date all regulatory authorities whether it is US-FDA or MHRA focused on the breach of data integrity especially they focus on the Laboratory data integrity and to prevent the breach of data integrity in the HPLC system we need to focus on the below-mentioned area/points.
- Individual User Name & Password on the system/software attached to the HPLC. There should be a password policy or system enabled policy which bound to change the password on each individual after a certain period and password should not be shared with anyone.
- System/software should have enabled audit trail and it should be reviewed for both system and project by competent reviewer at a defined period to identify any breach of procedure.
- There should be a different user group on systems like Analyst, Reviewer, Approver, Administrative who have different privileges access. The administrative should be an independent person, he should not be a Quality Control person. Rights to the user should be defined based on his/her competency level. The only Administrator should have rights for any deletion which should be pre-approved by Quality Assurance.
- Computer system should have locked date and time/ timezone field so that no-one can change the date & time of the computer system which can affect the final report.
- Any change in the policy needs to be authorized and to be done in a controlled way.
- Re-processing, Modification in results should be controlled and justified.
- Any gap observed during an audit trail review needs to evaluated and justified.
- Administrative rights usage to be controlled and monitored.
- Sequence, methods, results, and channels audit trails to be reviewed with each analysis.
So now you can understand how can you control breach of data integrity on the HPLC system used in the pharmaceutical & Healthcare Laboratory.