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Physical & Chemical properties

Stability in organic solvents and identity of relevant degradation products

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Reference
Endpoint:
stability in organic solvents and identity of relevant degradation products
Type of information:
experimental study
Adequacy of study:
key study
Study period:
20 November 2014 to 11 June 2015
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Qualifier:
no guideline available
Principles of method if other than guideline:
HPLC method using UV absorbance detection at a wavelength of 280 nm for determination of test material concentration and stability in peanut oil formulations.
GLP compliance:
yes
Test substance stable:
yes
Transformation products:
not measured

- Under the described chromatographic conditions, the retention time of the test item was approximately 4.8 minutes.

- The total analysis time for each run was 10.0 minutes.

- Assay specificity/selectivity was confirmed when HPLC/UV analysis of processed vehicle samples revealed no significant peaks (with S/N > 10) at or near the retention time for the test item.

- The post-storage test item concentrations ranged from 82.5 % to 93.4 % of the pre-storage values.

- For a nominal concentration of 1 mg/mL, mean concentration at time zero was determined to be 0.830 mg/mL (90.2 % of pre-storage value) after 5 days at room temperature.

- For a nominal concentration of 1 mg/mL, mean concentration at time zero was determined to be 0.735 mg/mL (82.5 % of pre-storage value) after 10 days at room temperature.

- For a nominal concentration of 250 mg/mL, mean concentration at time zero was determined to be 228 mg/mL (93.4 % of pre-storage value) after 5 days at room temperature.

- For a nominal concentration of 250 mg/mL, mean concentration at time zero was determined to be 212 mg/mL (86.8 % of pre-storage value) after 10 days at room temperature.

- Samples stored at room temperature for 10 days did not meet the acceptance criteria stated in the protocol for stability (i.e., the post-storage concentration was not 90 % of the pre-storage value).

Conclusions:
Formulations prepared in peanut oil at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for homogeneity and re-suspension homogeneity after 5 and 10 days storage at room temperature. The protocol-specified acceptance criteria for stability were met for formulations stored at room temperature for five days but not for samples stored at room temperature for 10 days.
Executive summary:

METHOD

Test item concentration from 1.00 to 250 mg/mL in peanut oil was determined using an HPLC method and UV absorbance at a wavelength of 280 nm.Test item stability was assessed in a QC stock solution stored at room temperature for a minimum of four days, in calibration standards, and in processed QC samples stored at room temperature for a minimum of 10 days. Test item homogeneity, re-suspension homogeneity and stability were assessed after 5 to 10 days storage at room temperature together for formulations prepared at target test item concentrations of 1 and 250 mg/mL

RESULTS

The test material assay procedure was validated in this study with 3 validation sessions. Quantitation was performed using calibration standards ranging in test item concentration from 20.0 to 200 μg/mL. The mean back-calculated standard concentrations had inter-session variability ranging from 0.81% to 7.9% Relative Standard Deviation (RSD) and % Relative Error (RE) ranging from -3.6% to 3.8%, which met the protocol-specified acceptance criteria for calibration standards, i.e., RSD ≤10% (≤15% at the lowest concentration) and %RE within ± 10% (± 15% at the lowest concentration). Assay precision and accuracy were verified by the analysis of QC samples prepared at nominal concentrations of 1.00, 50.0, and 250 mg test material/mL. The mean calculated QC concentrations had inter-session variability (precision) ranging from 2.0% to 8.5% RSD and %RE (accuracy) ranging from -5.3% to -3.1%, which met the protocol-specified acceptance criteria for precision and accuracy, i.e., RSD ≤ 15% and %RE within ± 15%.

With one exception where the mean concentration of the QC stock solution stored for a minimum of 4 days at room temperature was 79.9% of the target concentration, the test item in a QC stock solution stored at room temperature for a minimum of 4 days and in calibration standards and processed QC samples stored at room temperature for a minimum of 10 days met the proocol-specified acceptance criteria for stability (i.e., the post-storage concentration was not < 90% of the pre-storage value).

The results of test item homogeneity assessment in formulations prepared at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for homogeneity (i.e. the RSD for the mean concentration was ≤ 10% at a concentration within the acceptable limits (85 % to 115 % of target)). Assessment of test item resuspension homogeneity and stability in formulations prepared at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for resuspension homogeneity after 5 and 10 days of room temperature storage (i.e. the RSD for the mean concentration was ≤ 10%). The previously stated protocol-specified acceptance criteria for stability were met for formulations stored at room temperature for five days but not for samples stored at room temperature for 10 days.

Description of key information

Formulations prepared in peanut oil at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for homogeneity and re-suspension homogeneity after 5 and 10 days storage at room temperature. The protocol-specified acceptance criteria for stability were met for formulations stored at room temperature for five days but not for samples stored at room temperature for 10 days.

Additional information

METHOD

Test item concentration from 1.00 to 250 mg/mL in peanut oil was determined using an HPLC method and UV absorbance at a wavelength of 280 nm. Test item stability was assessed in a QC stock solution stored at room temperature for a minimum of four days, in calibration standards, and in processed QC samples stored at room temperature for a minimum of 10 days. Test item homogeneity, re-suspension homogeneity and stability were assessed after 5 to 10 days storage at room temperature together for formulations prepared at target test item concentrations of 1 and 250 mg/mL

RESULTS

The test material assay procedure was validated in this study with 3 validation sessions. Quantitation was performed using calibration standards ranging in test item concentration from 20.0 to 200 μg/mL. The mean back-calculated standard concentrations had inter-session variability ranging from 0.81% to 7.9% Relative Standard Deviation (RSD) and % Relative Error (RE) ranging from -3.6% to 3.8%, which met the protocol-specified acceptance criteria for calibration standards, i.e., RSD ≤10% (≤15% at the lowest concentration) and %RE within ± 10% (± 15% at the lowest concentration). Assay precision and accuracy were verified by the analysis of QC samples prepared at nominal concentrations of 1.00, 50.0, and 250 mg test material/mL. The mean calculated QC concentrations had inter-session variability (precision) ranging from 2.0% to 8.5% RSD and %RE (accuracy) ranging from -5.3% to -3.1%, which met the protocol-specified acceptance criteria for precision and accuracy, i.e., RSD ≤ 15% and %RE within ± 15%.

With one exception where the mean concentration of the QC stock solution stored for a minimum of 4 days at room temperature was 79.9% of the target concentration, the test item in a QC stock solution stored at room temperature for a minimum of 4 days and in calibration standards and processed QC samples stored at room temperature for a minimum of 10 days met the proocol-specified acceptance criteria for stability (i.e., the post-storage concentration was not < 90% of the pre-storage value).

The results of test item homogeneity assessment in formulations prepared at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for homogeneity (i.e. the RSD for the mean concentration was ≤ 10% at a concentration within the acceptable limits (85 % to 115 % of target)). Assessment of test item resuspension homogeneity and stability in formulations prepared at target concentrations of 1 and 250 mg test material/mL met the protocol-specified acceptance criteria for resuspension homogeneity after 5 and 10 days of room temperature storage (i.e. the RSD for the mean concentration was ≤ 10%). The previously stated protocol-specified acceptance criteria for stability were met for formulations stored at room temperature for five days but not for samples stored at room temperature for 10 days.