Analytical Instrument Qualification For HPLC System

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Analytical Instrument Qualification For HPLC System

1.0 Objective

To lay down a procedure for qualification of the Shimadzu HPLC system to ensure that the instrument is installed correctly, operates as intended, and consistently performs according to predefined specifications and regulatory requirements.

2.0 Scope

This procedure is applicable to qualification of Shimadzu High-Performance Liquid Chromatography (HPLC) systems installed in the Quality Control Laboratory.

3.0 Responsibility

3.1 Quality Control (QC) Officer/Executive

  • Preparation and execution of DQ, IQ, OQ, and PQ protocols

  • Documentation and compilation of qualification reports

3.2 Head – Quality Control

  • Review and approval of qualification documents

3.3 Quality Assurance (QA)

  • Verification of compliance with regulatory requirements

  • Final approval of qualification documents

3.4 Authorized Service Engineer (Shimadzu Representative)

  • Installation and operational support during qualification

4.0 Procedure

The Analytical Instrument Qualification shall be performed in four stages:

  • Design Qualification (DQ)

  • Installation Qualification (IQ)

  • Operational Qualification (OQ)

  • Performance Qualification (PQ)

4.1 Design Qualification (DQ)

4.1.1 Purpose

To ensure that the selected Shimadzu HPLC system is suitable for its intended analytical applications and complies with user requirement specifications (URS).

4.1.2 Procedure

a) System Requirement Verification
The following parameters shall be verified against URS:

  • Flow rate range

  • Detector sensitivity

  • Column compatibility

  • Software compliance and data management capability

Example Verification:

  • Required flow rate range: 0.001 to 10.0 mL/min

  • Shimadzu Nexera series capability: 0.0001 to 10.0 mL/min

  • Status: Complies

  • Required UV/Vis detector sensitivity: ≥ 0.5 × 10⁻⁵ AU

  • Shimadzu SPD-40 detector sensitivity: 0.4 × 10⁻⁵ AU

  • Status: Exceeds requirement

b) Compliance Assessment
Verification that the selected system meets regulatory requirements and laboratory standards.

c) Vendor Qualification
Evaluation of Shimadzu with respect to:

  • ISO certifications

  • After-sales service support

  • Availability of technical documentation

All findings shall be documented in the DQ report.

4.2 Installation Qualification (IQ)

4.2.1 Purpose

To verify and document that the Shimadzu HPLC system and its components are delivered, installed, and configured as per manufacturer specifications.

4.2.2 Procedure

a) Equipment Identification
Record:

  • Model number

  • Serial numbers

  • Software version

b) Component Verification
Verify installation of:

  • Pump

  • Autosampler (e.g., SIL-40)

  • Detector

  • Column oven

  • System controller

  • Software

Example:
Autosampler SIL-40 installed on [Date], Serial No. [XXXXXX], connectivity verified – Passed.

c) Environmental Condition Verification

  • Laboratory temperature: 20–25°C

  • Relative humidity: As per specification

  • Power supply: Stable and grounded

Example:
Temperature recorded at 22°C during installation – Complies.

d) Utility and Installation Checks

  • Proper plumbing connections

  • Electrical wiring verification

  • Software installation confirmation

All observations shall be recorded in the IQ report.

4.3 Operational Qualification (OQ)

4.3.1 Purpose

To verify that the HPLC system operates within specified operational limits.

4.3.2 Procedure

a) Pump Flow Rate Accuracy
Requirement: ±1% accuracy at 1.0 mL/min
Observed: 0.998 mL/min (0.2% deviation) – Passed

b) Detector Linearity
Requirement: R² ≥ 0.999 (0.1 to 1.0 AU range)
Observed: R² = 0.9993 – Passed

c) Column Oven Temperature Accuracy
Requirement: ±1°C of set point
Set Point: 40°C
Observed: 39.8°C to 40.1°C – Passed

d) System Suitability Test
Evaluate:

  • Resolution

  • Tailing factor

  • Theoretical plates

All data including chromatograms and calibration curves shall be attached to the OQ report.

4.4 Performance Qualification (PQ)

4.4.1 Purpose

To demonstrate that the Shimadzu HPLC system consistently performs according to intended analytical applications under routine laboratory conditions.

4.4.2 Procedure

a) Method-Based Performance Verification
Using a validated analytical method, evaluate:

  • Precision

  • Accuracy

  • Linearity

  • Limit of Detection (LOD)

  • Limit of Quantitation (LOQ)

  • Robustness

b) System Suitability Requirement
Resolution between two peaks ≥ 2.0
Observed: 2.5 – Passed

c) Precision
Requirement: RSD ≤ 2% for six injections
Observed: RSD = 1.4% – Passed

d) Accuracy (Recovery Study)
Requirement: 98–102%
Observed: 99.5%, 100.2%, 99.8% – Passed

e) Long-Term Stability Evaluation
Performance monitored over 7 days.
Result: No significant drift in retention time, peak area, or resolution – Passed

All chromatograms, raw data, and trend analysis shall be included in the PQ report.

5.0 Documentation

The final qualification report shall include:

  • Approved DQ, IQ, OQ, and PQ protocols

  • Raw data and observation sheets

  • Calibration certificates (if applicable)

  • Deviations and corrective actions (if any)

  • Summary report

6.0 Conclusion

Upon successful completion of DQ, IQ, OQ, and PQ, the Shimadzu HPLC system shall be considered qualified for routine analytical use.

The final report shall be reviewed and approved by:

  • QC Head

  • Quality Assurance

  • Authorized Shimadzu Service Representative

After approval, the instrument shall be released for routine laboratory analysis.

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