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Reference
Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
08 February 2017 - 08 February 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
EU Method C.19 (Estimation of the Adsorption Coefficient (KOC) on Soil and Sewage Sludge Using High Performance Liquid Chromatography (HPLC))
Deviations:
no
Qualifier:
according to
Guideline:
OECD Guideline 121 (Estimation of the Adsorption Coefficient (Koc) on Soil and on Sewage Sludge using High Performance Liquid Chromatography (HPLC))
Deviations:
no
Qualifier:
according to
Guideline:
other: European Commission (EC), Technical Guidance Document on Risk Assessment Part III, Chapter 4.3: “Use of (Quantitative) Structure Activity Relationships ((Q)SARs) - Soil and Sediment Sorption”, 2003.
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
HPLC estimation method
Media:
other: HPLC column
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Analytical purity: assay 101.1%
- Source and lot/batch No.of test material: M16FB2273
- Expiration date of the lot/batch: 2017-06-14 (retest date)
- Purity test date: 2016-09-19 (certificate of analysis release date)

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability under test conditions: stable
- Solubility and stability of the test substance in the solvent/vehicle: solubility in water: <0.1 g/L
Radiolabelling:
no
Test temperature:
35°C ± 1°C
Details on study design: HPLC method:
-Reference substance:4,4’-DDT

-Reference substance solution: A stock solution of 4,4’-DDT at concentrations of approximately 1 g/L in methanol was used. The stock solution was diluted to obtain an end solution of 55/45 (v/v) methanol/water. The blank solution for the reference substance was 55/45 (v/v) methanol/water.

-Test solution: A 1000 mg/L stock solution of the test item was prepared in methanol. In order to dissolve the test item the stock solution was ultrasonicated for 1 minutes. The stock solution was diluted to obtain an end solution of 55/45 (v/v) methanol/water. The final concentration of the test item solution was 10.0 mg/L. The test item blank solution was 55/45 (v/v) methanol/water.

-The reference substance and test item solutions were injected in duplicate. Blank solutions were analysed by single injection.

EQUIPMENT
- Apparatus: Acquity UPLC system (Waters, Milford, MA, USA)
- Type: Acquity UPLC PDA detector (Waters)
- Type, material and dimension of analytical (guard) column: Acquity UPLC HSS Cyano, 100 mm x 2.1 mm i.d., dp = 1.8 µm (Waters)
- Detection: 210 nm (UV)
- Column temperature: 35°C
-Flow: 0.4 mL/min
-Injection volume: 5 µL

MOBILE PHASES
- Type: 55/45 (v/v) methanol/water
- Solutes for dissolving test and reference substances:
- Reference substance solution: A stock solution of 4,4’-DDT at concentrations of approximately 1 g/L in methanol was used. The stock solution was diluted to obtain an end solution of 55/45 (v/v) methanol/water. The blank solution for the reference substance was 55/45 (v/v) methanol/water. -Test solution: A 1000 mg/L stock solution of the test item was prepared in methanol. In order to dissolve the test item the stock solution was ultrasonicated for 1 minutes. The stock solution was diluted to obtain an end solution of 55/45 (v/v) methanol/water. The final concentration of the test item solution was 10.0 mg/L. The test item blank solution was 55/45 (v/v) methanol/water.
- The reference substance and test item solutions were injected in duplicate. Blank solutions were analysed by single injection. The test item blank solution was 55/45 (v/v) methanol/0.01 M phosphate buffer pH 7.

REFERENCE SUBSTANCES
- Identity: 4,4'-DDT

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 10 mg/L.
- Quantity of reference substances: 1 g/L in methanol
- Intervals of calibration: no data

REPETITIONS
- Number of determinations: 2 times (test item solution), 1 time (blank solution)

EVALUATION
- Calculation of capacity factors k': from retention time of reference items, the test item, and then on-sorbed chemical item
- Determination of the log Koc value: a correlation of log k' versus log Koc of the reference items is plotted using linear regression - the log k' value of the test item is then used to calculate its log Koc value
Analytical monitoring:
no
Computational methods:
As per the guideline, the pKa values of the test item were calculated using the Perrin calculation method (pKalc 5.0, module in Pallas 3.0, CompuDrug International San Francisco, CA, USA). Based on the calculations, the UPLC analysis was performed at neutral pH.
Key result
Type:
Koc
Value:
> 430 000 dimensionless
pH:
7
Key result
Type:
log Koc
Value:
> 5.63 dimensionless
pH:
7
Details on results (HPLC method):
- Retention times (tr,1 and tr,2) of reference substances used for calibration:
* 4,4'-DDT: retention time (log Koc = 5.63) was 7.504 minutes.

- Details of fitted regression line (log k' vs. log Koc): none
- Average retention data for test substance: In the chromatogram of the test item solution, one peak with a retention time of 10.998 minutes was observed.
- Koc test substance = 2.2 x 10^5
Transformation products:
no
Validity criteria fulfilled:
yes
Conclusions:
The HPLC method using soil-adsorption-reference data was applied for the determination of the adsorption coefficient (Koc) of JNJ-42808389-AAA (T003421). No pKa values for acidic and basic groups in the molecular structure of the test item in the logarithm range of 1 - 14 were calculated. In the chromatogram of the test item solution, one peak with a retention time of 10.998 minutes was observed. Under the same analytical conditions, the retention time of 4,4’-DDT (log Koc = 5.63) was 7.504 minutes. Hence, it was concluded that the log Koc of test item was > 5.63 (Koc > 4.3E+5) at neutral pH.

Description of key information

In the guideline study (Ciric, 2017), the HPLC method using soil-adsorption-reference data was applied for the determination of the adsorption coefficient (Koc) of JNJ-42808389-AAA (T003421). The Koc and log Koc values of the test item at neutral pH were >4.3E+5 and >5.63 respectively. Results of this study are considered reliable without restriction.

Key value for chemical safety assessment

Koc at 20 °C:
430 000

Additional information

[LogKoc: 5.63]