Moisture Content and Stability-Critical Range Validation in Oral Granules for Suspension Manufacturing

All equipment used in this process validation must be duly qualified and validated for its intended use and performance specifications. Equipment qualification (IQ/OQ/PQ) is assumed to be completed prior to this process validation.

Defining Quality Target Product Profile (QTPP) for Oral Granules

Step 1: Clearly outline the QTPP attributes related to oral granules for suspension, specifically focusing on moisture-related parameters such as residual moisture limits that affect flowability, uniformity, and reconstitution time.

Step 2: Ensure the QTPP includes the expected stability duration, desired pharmacotechnical characteristics, and microbial limits influenced by moisture content.

Step 3: Align the QTPP with regulatory guidelines and product-specific requirements to establish a benchmark for validating moisture content.

Desired Attributes of Moisture Content in Oral Granules

Step 1: Identify target moisture levels that maintain granule integrity without promoting caking or excessive dryness, which could affect the suspension quality.

Step 2: Select appropriate moisture measurement methods such as Karl Fischer titration, loss on drying (LOD), or near-infrared (NIR) spectroscopy that provide precise, reproducible results aligned with the dosage form’s characteristics.

Step 3: Incorporate moisture specifications into product release criteria ensuring consistency with validated ranges.

Impact of Moisture Content on QTPP

Step 1: Analyze how deviations in moisture content can alter critical performance attributes such as dissolution rate, dose uniformity, sedimentation behavior, and microbial growth potential.

Step 2: Utilize stability studies to demonstrate the relationship between moisture variation and resultant changes in product quality over shelf life.

Step 3: Define acceptable moisture thresholds that do not compromise the QTPP attributes to ensure patient safety and efficacy.

Critical Quality Attributes (CQAs) Related to Moisture Content and Stability

Step 1: Identify CQAs directly affected by moisture including flow properties, particle size distribution, reconstitution time, and microbial bioburden.

Step 2: Develop assays and monitoring protocols to measure these CQAs routinely during process validation and continued manufacturing.

Step 3: Correlate moisture content limits with CQA acceptance criteria to establish a stability-critical range that consistently meets quality standards.

Key Properties of Oral Granules for Suspension Affecting Stability

Step 1: Assess granule physicochemical properties such as porosity, hardness, and surface area that influence moisture absorption and retention.

Step 2: Evaluate packaging materials and environmental conditions that can impact moisture ingress and granule stability during storage.

Step 3: Implement process control strategies, including controlled drying and environmental monitoring, to maintain these key properties within validated parameters.

Risk Assessment and Failure Mode Effects Analysis (FMEA) for Moisture Content and Stability-Critical Range Validation

Begin by conducting a comprehensive Risk Assessment and FMEA focused on moisture content and stability-critical parameters in the manufacturing of oral granules for suspension. Identify critical failure points that could adversely affect granule quality, specifically moisture-related degradation, caking, or dissolution issues.

1. List potential failure modes such as excessive moisture uptake, inadequate drying, and granule agglomeration.
2. Evaluate severity, occurrence, and detectability for each failure mode. For example:
   • Severity: High if moisture affects API stability or suspension uniformity.
   • Occurrence: Medium to high during drying or environment exposure.
   • Detectability: Moderate depending on monitoring techniques in place.
3. Calculate Risk Priority Numbers (RPN) to prioritize control focus.
4. Document all findings and integrate risk mitigation plans into subsequent process steps.

Design of Experiments (DoE) for Identification of Critical Process Parameters (CPPs)

Execute a structured DoE to identify and quantify the impact of process parameters on moisture content and stability-critical ranges. This step is essential to establish robust process control.

1. Select process factors, including drying temperature, drying time, humidity control, and granule blending intensity.
2. Define response variables such as residual moisture percentage, moisture distribution uniformity, and stability indicators over predefined storage conditions.
3. Design factorial or response surface methodology (RSM)-based DoE with sufficient runs to capture interactions.
4. Perform experimental batches per DoE matrix under controlled environmental conditions.
5. Analyze data to identify statistically significant CPPs affecting moisture and stability.

Critical Process Parameter (CPP) Selection and Justification

Based on DoE outcomes, finalize the list of CPPs specifically impacting moisture content and granule stability as critical quality attributes (CQAs).

1. Highlight parameters such as drying temperature (e.g., 40–60°C), drying time (e.g., 30–90 minutes), and humidity control during packaging as CPPs.
2. Ensure each CPP is linked to its impact on moisture critical ranges and ultimate product stability.
3. Provide rationale for exclusion of non-significant factors to maintain process efficiency.

Establishment of Control Strategy and Acceptable Range Definition

Develop an integrated control strategy to maintain moisture content and stability within validated limits throughout manufacturing and storage.

1. Establish acceptable moisture content range based on stability data, typically defined as percent moisture below a threshold that ensures product integrity (e.g., 2.0%–3.5%).
2. Define control limits for CPPs, such as specific drying temperature and time windows proven to yield consistent moisture levels.
3. Incorporate in-process controls such as near-infrared (NIR) spectroscopy or loss on drying (LOD) tests conducted at critical points.
4. Implement environmental controls for manufacturing and packaging areas to maintain relative humidity below critical thresholds (e.g., <40%).

Process Flow and Stepwise Workflow to Monitor Moisture and Stability

Outline the detailed process flow emphasizing moisture control checkpoints and stability assurance steps:

1. Raw Material Receipt and Storage: Ensure raw materials are stored in low-humidity environments. Sample and test incoming excipients for moisture levels.
2. Granulation: Monitor water addition closely; maintain process parameters to avoid excessive moisture.
3. Drying Stage: Control drying parameters tightly. Use calibrated moisture analyzers onsite for real-time assessments at the end of drying.
4. Post-Drying Blending: Minimize granule exposure to ambient humidity by operating in climate-controlled rooms or inert atmospheres.
5. Packaging: Use moisture barrier packaging materials and control packaging environment humidity.

Sampling and Decision Points for Moisture Content Verification

Implement a sampling plan integrated within the manufacturing workflow to verify moisture content and stability-critical parameters in-process and post-process.

1. Define sampling locations and frequency — for example, samples taken immediately after drying, post-blending, and pre-packaging.
2. Utilize validated analytical methods such as Loss on Drying (LOD) or Karl Fischer titration for moisture determination.
3. If moisture levels fall outside acceptable range, activate predefined deviation protocols, which may include reprocessing or batch rejection.
4. Record all sampling results and decisions in a batch manufacturing record (BMR) for traceability and regulatory compliance.

Process Performance Qualification (PPQ) and Protocol Design

Following development and control strategy establishment, design and execute Process Performance Qualification batches to demonstrate consistent control over moisture content and critical stability attributes.

1. Develop a detailed PPQ protocol that includes:
   • Defined CPP setpoints and ranges established from prior DoE and validation studies.
   • Sampling plans for in-process and finished product moisture tests.
   • Acceptance criteria aligned with stability data and product specifications.
   • Methods to document and investigate any nonconformities.
   • Environmental monitoring and control requirements during manufacturing.
2. Manufacture at least three consecutive batches under the defined conditions to confirm process reproducibility.
3. Perform moisture content and stability tests on PPQ batches, including accelerated and long-term stability assessments.
4. Conduct statistical evaluation of PPQ data to confirm capability and control.
5. Prepare a comprehensive PPQ report summarizing results, deviations, and conclusions.

Batch Execution, Evaluation, and Continuous Monitoring

Execution of batch manufacturing during validation must adhere strictly to protocol specifics, with continuous evaluation for compliance with moisture and stability criteria.

1. Ensure all operators are trained on critical control points and sampling procedures.
2. Perform real-time moisture measurements during production, triggering corrective actions if deviations occur.
3. Log environmental parameters such as humidity and temperature to ensure consistency during processing and packaging.
4. After batch completion, evaluate all analytical data, deviations, and in-process controls specific to moisture and stability.
5. Confirm that validated moisture content ranges are consistently met, and stability testing demonstrates no adverse impact on product quality.
6. Implement continuous monitoring programs post-validation to detect process drift or environmental changes affecting moisture control.

Control Strategy for Moisture Content and Stability

Develop a comprehensive control strategy to maintain moisture content and stability within validated critical ranges:

• In-Process Monitoring: Continuously monitor drying temperature and time using calibrated sensors to ensure parameters remain within CPP limits.
• Environmental Controls: Maintain relative humidity in manufacturing and packaging areas within specified limits to prevent moisture uptake post-drying.
• Granule Handling: Minimize exposure of granules to ambient conditions during transfer by using closed or controlled systems.
• Packaging: Validate moisture barrier properties of packaging materials and control packaging environment humidity to maintain granule stability.

Establishment of Acceptable Ranges and Monitoring Plan

Define acceptable ranges for moisture content and stability-critical parameters based on risk assessment, DoE, and historical data:

• Set residual moisture content range, for example, 2.0%-3.5% w/w, aligned with optimal stability and suspension performance.
• Define tolerances for drying temperature and time within the validated CPP ranges (e.g., 40–60°C for temperature, 30–90 minutes for drying duration).
• Institute routine sampling intervals during drying and post-drying stages for moisture content measurement using validated analytical methods.
• Implement trending analysis on moisture levels and stability indicators to detect shifts or trends outside control limits.

Stepwise Process Flow and Sampling Strategy

Outline detailed workflow steps incorporating critical sampling and decision points:

1. Granule Preparation: Record batch details and initial moisture baseline.
2. Drying Step: Initiate drying under preset CPPs; collect moisture content samples at mid-point and end of drying process.
3. Post-Drying Assessment: Analyze samples to confirm moisture content within validated range before proceeding.
4. Blending: Monitor granule uniformity and saturation levels if applicable.
5. Packaging: Sample finalized granules for post-packaging moisture verification.
6. Storage Stability Testing: Conduct accelerated and long-term stability studies on representative samples.

Process Performance Qualification (PPQ) and Protocol Design

Design the PPQ protocol to confirm consistent process performance within validated conditions:

• Batch Selection: Select consecutive commercial-scale batches representing typical process variables.
• Data Collection: Record all CPP and CQA parameters, including moisture content, drying conditions, and environmental factors.
• Acceptance Criteria: Define pass/fail criteria based on validated moisture and stability ranges.
• Deviation Management: Outline procedures for investigation and documentation of excursions beyond acceptable ranges.
• Outcome Evaluation: Analyze PPQ data statistically to confirm process reproducibility and compliance.

Batch Execution and Evaluation

Implement process validation batches as per the approved PPQ protocol:

• Execute manufacturing and drying steps with real-time monitoring and adherence to CPPs.
• Collect moisture content data at predefined sampling points; verify results meet acceptance criteria before progressing.
• Document deviations and corrective actions taken promptly during batch processing.
• Perform post-batch stability assessments to ensure granule integrity and suspension performance are retained.
• Compile batch records and validation reports summarizing compliance to validated moisture content and stability-critical ranges.

Control Strategy Development for Moisture Content and Stability-Critical Ranges

Develop a comprehensive control strategy encompassing all identified CPPs to maintain moisture within the established stability-critical range:

• Implement real-time moisture monitoring using near-infrared (NIR) spectroscopy or loss-on-drying techniques at key stages.
• Control drying parameters tightly, setting advanced alarms or automatic cut-offs when moisture deviates from set limits.
• Establish environmental controls for manufacturing and packaging areas to maintain relative humidity within acceptable levels (e.g., ≤50%).
• Include standardized procedures for granule blending to ensure uniform moisture distribution.
• Integrate control charts for continuous trending of moisture data across batches to detect trends and shifts.

Specification of Acceptable Moisture Content Ranges

Define clear acceptance criteria based on stability studies and regulatory guidance:

• Set residual moisture target range, e.g., 1.5%–3.5% w/w, ensuring product stability and suspensibility.
• Allow narrow tolerance windows around target ranges, justified by empirical product performance data.
• Specify limits for moisture variability between multiple samples within each batch (e.g., ±0.2%).

Sampling and Monitoring Points in Process Flow

Establish critical sampling points in the manufacturing workflow to verify moisture content:

1. Immediately post-drying before granule conditioning to confirm drying efficacy.
2. Post-blending to ensure moisture uniformity throughout the batch.
3. Pre-packaging sampling to validate moisture stability before sealing.
4. Frequency: Initially every batch for PPQ and periodically as per ongoing process verification.

Process Performance Qualification (PPQ) Protocol Design

Design the PPQ protocol to confirm that process consistently produces granules within moisture and stability specifications:

• Include at least three consecutive commercial-scale batches to demonstrate reproducibility.
• Detail sampling plans at critical control points with specified sample sizes and acceptance criteria.
• Incorporate testing for moisture content, uniformity, and stability indicators throughout shelf life.
• Define escalation actions if batches fall outside acceptable moisture ranges, including investigation and root cause analysis.
• Document batch manufacturing parameters, environmental conditions, and instrumentation calibration status.

Batch Execution and Comprehensive Evaluation

Execute PPQ batches in strict accordance with the validation protocol and established control strategy:

• Perform real-time monitoring of CPPs and moisture measurements as specified.
• Record all data with full traceability including equipment IDs, operator actions, and deviations.
• Evaluate moisture results statistically against acceptance criteria and target stability ranges.
• Assess the correlation between process parameters and moisture content to confirm CPP control effectiveness.
• Generate a detailed validation report summarizing findings, deviations, and confirming process capability.

Development of Control Strategy and Establishment of Acceptable Ranges

Develop a comprehensive control strategy to maintain moisture content and stability within validated critical ranges during the manufacturing of oral granules for suspension.

• Define acceptable moisture content limits based on DoE and stability data, for example, residual moisture range of 2.0% to 5.0% w/w.
• Integrate environmental controls such as temperature and relative humidity set points in manufacturing and packaging areas.
• Implement in-process controls including real-time moisture monitoring with loss-on-drying (LOD) or near-infrared (NIR) technology.
• Establish feedback loops to adjust drying cycle parameters dynamically if moisture deviation is detected.
• Specify packaging material requirements that mitigate moisture ingress post-manufacturing.
• Document acceptance criteria for finished granules before release and suspension reconstitution.

Process Monitoring and Sampling Strategy

Outline a systematic monitoring and sampling framework throughout the granule manufacturing process to ensure maintenance within validated moisture and stability limits.

• Define critical sampling points, for example:
• Post-drying granules to assess residual moisture.
• Pre-packaging to verify granule stability and moisture uniformity.
• Final packaged product to confirm moisture barrier integrity.
• Determine sampling frequency based on process variability and risk assessment, e.g., every batch or every nth batch depending on historical data.
• Standardize sampling techniques to minimize variability and ensure representative samples.
• Specify analytical methods validated for accuracy and precision in moisture measurement.
• Use trending and statistical process control charts to monitor data over time and trigger investigations if trends approach control limits.

Process Performance Qualification (PPQ) Protocol Design

Design the PPQ protocol to confirm that the oral granules manufacturing process consistently meets moisture and stability specifications under commercial-scale conditions.

• Define batch size, number of consecutive batches (minimum three), and manufacturing conditions reflecting routine commercial process.
• Include planned sampling points aligned with the sampling strategy for all identified CPPs.
• Specify acceptance criteria for moisture content, granule stability, and physical attributes.
• Outline the test methods, equipment calibration requirements, and data handling procedures.
• Include contingency plans for excursions such as out-of-specification moisture content or physical instability.
• Detail documentation and approval workflows for process deviations and corrective actions.

Batch Execution and Data Evaluation

Execute the PPQ batches according to the approved protocol, ensuring strict adherence to process parameters and control strategy.

• Monitor and record all CPPs continuously with calibrated instruments.
• Collect samples at specified process points for moisture and stability analysis.
• Evaluate moisture content results against acceptable ranges; identify any deviations and investigate root causes.
• Assess stability data for product performance through predefined time points under accelerated and long-term storage conditions.
• Compile process data, trend analyses, and stability outcomes into a comprehensive PPQ report.
• Confirm process capability and robustness ensuring consistent production of oral granules within validated moisture and stability ranges.
• Recommend process adjustments or improvements as necessary based on batch evaluation.

Control Strategy Development

Establish a comprehensive control strategy to maintain moisture content within the validated critical range and ensure granule stability throughout the manufacturing process.

• Define acceptable moisture content ranges based on stability studies and DoE results, e.g., 2.5–4.0% w/w residual moisture.
• Implement environmental controls such as humidity-controlled manufacturing and packaging areas.
• Incorporate in-process controls including real-time moisture measurement via near-infrared spectroscopy (NIR) or loss on drying (LOD) at key manufacturing steps (e.g., post-drying, post-milling).
• Set alert and action limits for each CPP to trigger corrective actions before batch deviation.
• Design packaging controls to minimize moisture ingress during storage and shipment.

Process Flow and Stepwise Workflow

Detail the validation process flow focussing on critical moisture and stability control points in oral granules manufacture.

1. Raw Material Receipt and Pre-check: Confirm incoming excipients and APIs meet moisture specifications.
2. Granulation and Drying: Apply validated drying parameters; monitor moisture content immediately post-drying.
3. Milling and Sieving: Monitor granule integrity and moisture retention.
4. Blending: Ensure uniform moisture distribution; verify with frequent sampling.
5. Packaging: Execute moisture barrier packaging in controlled humidity; inline moisture checks.
6. Storage and Stability Conditioning: Store at validated conditions; periodically test moisture and physical stability.

Sampling and Decision Points

Define robust sampling plans and decision criteria to verify moisture content and stability at critical stages.

• Sample granules immediately after drying and after blending for moisture and physical tests (e.g., 3 samples per batch at defined locations).
• Use statistical sampling methods aligned with batch size and process variability.
• Apply pre-established acceptance criteria for moisture and physical attributes; borderline or failed results trigger re-processing or batch rejection.
• Implement trending analysis of moisture data to detect process drifts.

Process Performance Qualification (PPQ) Protocol Design

Design a PPQ protocol that rigorously challenges the process under commercial scale and confirms control of moisture content and stability.

• Define PPQ batch sizes reflecting commercial scale production.
• Include comprehensive in-process and final product testing for residual moisture and stability markers at multiple time points.
• Document CPP values, process conditions, and environmental parameters monitored continuously.
• Specify acceptance criteria for critical quality attributes and CPPs based on prior validation and DoE.
• Outline corrective and preventive action plans for deviations.

Batch Execution and Evaluation

Execute PPQ batches as per protocol and evaluate process consistency and product quality concerning moisture and stability.

• Record all CPPs and environmental conditions in real-time.
• Perform immediate moisture testing post critical steps; compare data against control limits.
• Monitor granule stability over defined storage periods with periodic moisture and dissolution testing.
• Analyze batch data statistically to confirm process capability (e.g., Cp, Cpk) and robustness.
• Compile final validation report summarizing performance, deviations, and conclusions on validated moisture content and stability-critical ranges.

Introduction to Moisture Content and Stability-Critical Range Validation in Oral Granules for Suspension

When manufacturing oral granules for suspension, tightly controlled moisture content is vital for product stability, uniformity, and performance. This process validation outlines the stepwise approach to establishing, verifying, and documenting the moisture content critical range—with a focus on ensuring optimal stability throughout manufacturing and shelf life.

All equipment involved in moisture measurement and granule drying must have completed installation qualification (IQ), operational qualification (OQ), and performance qualification (PQ) prior to commencing process validation activities.

Define Critical Quality Attributes (CQAs) and Critical Process Parameters (CPPs)

1. Identify moisture content as a CQA for oral granules, directly influencing suspension stability and redispersibility.
2. Establish the initial target moisture content range based on formulation development, literature, and prior stability studies (e.g., 2.5%–4.5% w/w moisture).
3. Characterize CPPs impacting moisture content, such as drying time, drying temperature, and granule sieve size distribution.

Select and Validate Moisture Determination Methods

1. Choose an appropriate moisture measurement technique (e.g., Loss on Drying (LOD) by Karl Fischer titration or moisture analyzer), ensuring sensitivity and specificity relevant to granule matrix.
2. Perform method validation covering accuracy, precision, linearity, and robustness according to ICH Q2(R1) guidelines.
3. Document method validation data within Annexure I: Moisture Content Method Validation Template.

Process Validation Batch Manufacturing and Moisture Content Testing

1. Manufacture at least three consecutive validation batches under controlled conditions following the validated process parameters.
2. At each batch, perform in-process moisture sampling at defined stages (post-granulation, post-drying) to assess adherence to specified moisture ranges.
3. Use validated moisture testing method and ensure repeatability through triplicate measurements per sample.
4. Record all moisture content data with batch number, sampling time, and environmental conditions in Annexure II: Moisture Content Batch Data Sheet.

Data Verification and Compliance Analysis

1. Compile moisture content values for all three validation batches into a Validation Results Table.

Batch Number	Sampling Point	Measured Moisture Content (%)	Method Replicates (n=3) – Mean ± SD	Compliance (Pass/Fail)
Batch 1	Post-Drying	3.8%, 3.9%, 3.7%	3.8 ± 0.1	Pass
Batch 2	Post-Drying	3.6%, 3.7%, 3.7%	3.67 ± 0.06	Pass
Batch 3	Post-Drying	4.0%, 3.9%, 4.1%	4.0 ± 0.1	Pass

2. Calculate the Relative Standard Deviation (RSD) for moisture content across batches to assess process consistency:
   RSD (%) = (Standard Deviation / Mean) × 100
3. Acceptable RSD for moisture in granules is typically ≤2%. In this example, RSD = 5.4% with a scope to investigate tighter process controls.

Comparative Summary of Moisture Content and Stability Impact

From the comparative summary, batches maintaining moisture within 3.5–4.2% demonstrate acceptable stability and performance, confirming the critical range.

Routine Monitoring and CPV Documentation

1. In routine production, perform moisture content testing on a minimum of 10% of batches or every batch depending on risk assessment.
2. Establish trending and statistical process control (SPC) charts for moisture content over time as part of Annual Product Quality Review (APQR).
3. Document all routine monitoring results with annotations for any deviations in Annexure III: Moisture Content Routine Monitoring Log.
4. Any out-of-specification (OOS) results require investigation and corrective action documented in Annexure IV: OOS Investigation and CAPA Template.

Stability-Critical Range Confirmation During Stability Studies

1. Confirm moisture content stability through long-term and accelerated stability studies on representative batches.
2. Measure moisture content at predefined intervals per stability protocol and correlate with product efficacy and physical attributes.
3. Update the validated moisture critical range if shifts occur while maintaining product quality.
4. Results and assessments to be recorded in Annexure V: Moisture Content Stability Study Report Template.

Annexures Summary

• Annexure I: Moisture Content Method Validation Template – Includes method protocol, validation data, and approval.
• Annexure II: Moisture Content Batch Data Sheet – Raw data capturing for each validation batch.
• Annexure III: Moisture Content Routine Monitoring Log – Used for in-process and routine checks post-validation.
• Annexure IV: OOS Investigation and CAPA Template – Investigation and corrective action documentation.
• Annexure V: Moisture Content Stability Study Report Template – To document long-term stability confirming critical range.

Adhering to these validation steps ensures robust control over moisture content, safeguarding the physical stability and quality of oral granules for suspension formulations. Proper documentation and ongoing monitoring maintain compliance with regulatory expectations and support continuous improvement.

Data Verification and Compliance Analysis (Continued)

Compile moisture content values for all three validation batches and perform statistical analysis to verify compliance with the established critical range.

• Calculate mean moisture content, standard deviation (SD), and relative standard deviation (RSD) for intra-batch and inter-batch variability.
• Analyze compliance against the acceptance criteria (e.g., moisture within 2.5%–4.5% w/w for ≥95% of samples).
• Evaluate optimum moisture content that ensures stability and minimizes degradation, supported by trending data.

Comparative Summary of Moisture Content Across Validation Batches

Provide a comparative summary that highlights consistency and stability of moisture content across all validation batches, emphasizing process reproducibility and robustness.

Continuous Process Verification (CPV) and Routine Monitoring

Establish procedures for ongoing monitoring of moisture content to ensure sustained control over the process post-validation.

1. Implement routine moisture content testing with defined sampling frequency (e.g., every production batch).
2. Use control charts to monitor moisture trends and detect deviations or shifts from the validated range.
3. Define criteria for escalation and investigation if moisture content is trending toward out-of-specification (OOS) limits.
4. Document all routine monitoring results in Annexure III: Moisture Content Routine Monitoring Log.

Trending Analysis and Annual Product Quality Review (APQR)

Ensure moisture content data are integrated into the APQR report to support ongoing product quality and demonstrate process stability over time.

1. Compile moisture content data across batches produced within the review period.
2. Perform statistical trending, including calculation of RSD, mean, and any significant excursions or outliers.
3. Summarize findings in APQR to confirm ongoing compliance with moisture critical range and process stability.
4. Review and update critical range or process parameters if necessary based on trending insights.

Annexures: Templates for Documentation and Records

For thorough documentation, utilize the following annexure templates to ensure traceability and regulatory compliance throughout the validation lifecycle:

• Annexure I: Moisture Content Method Validation Template – Method validation data and acceptance criteria.
• Annexure II: Moisture Content Batch Data Sheet – Raw data recording for each batch’s moisture measurements.
• Annexure III: Moisture Content Routine Monitoring Log – Ongoing routine control chart and batch test records.
• Annexure IV: CPV Compliance Checklist – Checklist for continuous verification protocols and compliance status.
• Annexure V: Moisture Content Trending Summary for APQR – Data consolidation template for trending analysis and report integration.