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Reference
Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2016-06-09 to 2016-06-09
Reliability:
1 (reliable without restriction)
Qualifier:
according to guideline
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
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
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
Type of method:
HPLC estimation method
Media:
other: HPLC column
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: I15FB3131
- Expiration date of the lot/batch: 11 June 2017
- Purity: 100% (based on assay base titration)
- Purity test date: 2015-09-04

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
Radiolabelling:
no
Test temperature:
column temperature 35°C ± 1°C
Details on study design: HPLC method:
EQUIPMENT:
- Instrument: Acquity UPLC system (Waters, Milford, MA, USA)
- Detector: Acquity UPLC PDA detector (Waters)
- Column: Acquity UPLC HSS Cyano, 100 mm  2.1 mm i.d., dp = 1.8 µm (Waters)
- Column temperature: 35°C +/-1°C
- Mobile phase: 55/45 (v/v) methanol/water
- Flow: 0.4 mL/min
- Injection volume: 5 µL
- UV detection: 210 nm

MOBILE PHASES
- Type: Stock solutions of the reference substances at concentrations of approximately 1 g/L in methanol were used. The stock solutions were diluted to obtain an end solution 55/45 (v/v) methanol/water.
- Solutes for dissolving test and reference substances:
* Solution of the unretained compound: A 5.0 g/L stock solution of formamide (99.2%, [75-12-7], Alfa Aesar, Karlsruhe, Germany) in methanol was used. The stock solution was diluted to obtain an end solution of 55/45 (v/v) methanol/water.
* Reference substance solutions: Stock solutions of the reference substances at concentrations of approximately 1 g/L in methanol were used. The stock solutions were diluted to obtain an end solution 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 5 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. In order to prevent any degradation, the time between dilution of the stock solution and UPLC analysis was kept as short as possible.

REFERENCE SUBSTANCES
- Identity: Acetanilide; Monuron; 2,5-Dichloroaniline; Naphthalene; Benzoic acid phenylester; Fenthion; Phenanthrene; 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
- Intervals of calibration: no data

REPETITIONS
- Number of determinations: The reference substance and test item solutions were injected in duplicate. Blank solutions were analysed by single injection.

EVALUATION
- Calculation of capacity factors k': from retention time of reference items, the test item, and the onsorbed chemical item.
- Calculation of retention times:
- 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
Key result
Type:
Koc
Value:
5.9 dimensionless
pH:
7
Remarks on result:
other: extrapolated value
Key result
Type:
log Koc
Value:
0.77 dimensionless
pH:
7
Remarks on result:
other: extrapolated results
Details on results (HPLC method):
- retention times (tr1 and tr2) of reference substances used for calibration:
*Formamide (t0) : tr1 = 0.670 min; tr2= 0.670 min
* Acetanilide : tr1 = 0.889 min; tr2= 0.885 min
* Monuron: tr1 = 1.101min;tr2= 1.097min
* 2,5-Dichloroaniline: tr1 = 1.266min;tr2= 1.265min
* Naphthalene: tr1 = 1.476min;tr2= 1.473min
* Benzoic acid phenylester:tr1 = 1.747min;tr2= 1.734min
* Fenthion:tr1 = 2.357min;tr2= 2.357min
* Phenanthrene: tr1 = 2.612min;tr2= 2.603min
* 4,4’-DDT:tr1 = 6.544min;tr2= 6.551min
- The equation of the regression line was: log k’ = 0.324 x log Koc – 0.822 (r = 0.98, n = 16)
- Mean retention time of test item: 0.85 min

The following pKa values in the logarithm range of 1 – 14 for acidic and basic groups in the molecular structure of the test item were calculated using the Perrin calculation method.

Calculated pKa values of the test item:

Phenol (Acidic): pKa 9.89

RARN(R1R2) (Basic): pKa 4.41

Based on the calculations, the UPLC analysis was performed at neutral pH.

Validity criteria fulfilled:
yes
Conclusions:
The HPLC method using soil-adsorption-reference data (OECD 121) was applied for the determination of the adsorption coefficient (Koc) of the test item of JNJ-119379-AAA (T001141). The Koc and log Koc values of the test item were 5.9 and 0.77 respectively. The results of the test can be considered reliable without restriction.

Description of key information

Based on the results of the guideline study (Reingruber, 2016), it is concluded that the Koc and log Koc values of the test item, JNJ-119379-AAA (T001141) were 0.59 and 0.77 respectively. The results of this study are reliable without restriction.

Key value for chemical safety assessment

Koc at 20 °C:
5.9

Additional information

[LogKoc: 0.77]