(4aR*,8aR*)-1-bromo-4a,5,9,10,11,12-hexahydro-3-methoxy-11-methyl-6H-benzofuro[3a,3,2-ef][2]benzazepin-6-one hydrochloride

Adsorption / desorption

Administrative data

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2002-07-12 to 2002-08-26

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2002

Report date:

2002

Materials and methods

Test guideline

Test guideline 1

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

Test guideline 2

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

GLP compliance:

yes (incl. QA statement)

Type of method:

HPLC estimation method

Media:

other: HPLC column

Test material

Test material information

Constituent 1

Reference substance name:

-

EC Number:

439-750-2

EC Name:

-

Cas Number:

183487-56-1

Molecular formula:

Hill formula: C17H19BrClNO3 CAS formula: C17H19BrClNO3

IUPAC Name:

(14S)-4-bromo-2-methoxy-7-methyl-17-oxa-7-azatetracyclo[12.2.1.0^{5,16}.0^{10,15}]heptadeca-1,3,5(16),10-tetraen-12-one hydrochloride

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Details on test material:

- Name of test material (as cited in study report): TIC2782 - T002907
- Physical state: white solid
- Analytical purity: 92.8%
- Lot/batch No.: RT002113G3A231
- Expiration date of the lot/batch: August 2003
- Stability under test conditions: stable
- Storage condition of test material: at room temperature, ~20°C.

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: RT00211G3A231
- Expiration date of the lot/batch: 2001-12-01 (retest date)
- Purity test date: no data

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature at about 20°C
- Stability under test conditions: no data
- Solubility and stability of the test substance in the solvent/vehicle: no data

Radiolabelling:

no

Study design

Test temperature:

Column temperature 20°C

HPLC method

Details on study design: HPLC method:

EQUIPMENT
- Apparatus: Varian Pump 9010, Varian Autosampler 9100, Varian Detector 9050, Gynkotek Column Oven STH-585.
- Type: HPLC with UV-VIS detector, reversed phase column and aqueous mobile phase.
- Type, material and dimension of analytical (guard) column: LiChrospher 100 CN, particle size 5 µm, 250 mm - 4.6 mm.
- Detection: 235 nm for test substance, 210 nm for reference items and sodium nitrate

MOBILE PHASES
- Type: 0.06 N sulfuric acid and methanol (45:55; v/v)
- pH: 2.2
- Solutes for dissolving test and reference substances:
* Test solution: T002113 was dissolved in 10 mL of a mixture of acetonitrile and water (1:1; v/v) to prepare a stock solution of 2200 µg/L. The stock solution (100 µL) was diluted with a solvent mixture of 0.06 N sulfuric acid in methanol (45:55; v/V) to 10 mL to obtain a standard solution of 22 µg/L..
* Reference substance solutions: in methanol for the stock solutions of the reference items. A combined reference solution was prepared by transferring a certain amount of the different stock solutions into one volumetric flask and dilutng to a volume of 10 mL with a mixture of 0.06 N sulfurinc acid and methanol (45:55; v/v).

DETERMINATION OF DEAD TIME
- Method: by inert substances which are not retained by the column (sodium nitrate)

REFERENCE SUBSTANCES
- Identity: combined reference solution containing acetanilide, isoproturon, linuron, naphtalene, pyrazophos, diclofop-methyl.

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 10 mL of a 22 µg/mL solution (100 µL) diluted in solvent mixture of 0.06 N sulfuric acid and methanol (45:55; v/v).
- Quantity of reference substances: 10 mL of the combined reference solution (solvent mixture of 0.06 N sulfuric acid and methanol (45:55; v/v))
- Intervals of calibration: no data

REPETITIONS
- Number of determinations: 3 times (test item solution), 6 times (combined reference solution), 2 times (unretarded item solution)

EVALUATION
- Calculation of capacity factors k': from retention time of reference items, the test item, and the unretarded 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

Results and discussion

Adsorption coefficient

Adsorption coefficient 1

Key result

Type:

log Koc

Value:

2.9

Temp.:

20 °C

Remarks on result:

other: mean of 3 analyses

Adsorption coefficient 2

Key result

Type:

Koc

Value:

823

Temp.:

20 °C

Remarks on result:

other: mean of 3 analyses

Results: HPLC method

Details on results (HPLC method):

- Retention times of reference substances used for calibration:
* Acetanilide: 4.283-4.292 min.
* Isoproturon: 5.085-5.095 min.
* Linuron: 6.730-6.741 min.
* Naphtalene: 7.426-7.439 min.
* Pyrazophos: 9.145-9.168 min.
* Diclofop-methyl: 11.213-11.247 min.
- Details of fitted regression line (log k' vs. log Koc): slope = 0.249, y-axis intercept = -0.521, coefficient of regression = 0.987
- Average retention data for test substance: ~7.15 min
- Koc value of test substance = 823

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

The HPLC method using soil-adsorption-reference data was applied for the determination of the adsorption coefficient (Koc) of T002113.The mean log Koc of T002113 was determined to be 2.9 using the HPLC estimation method according to OECD guideline 121. These results indicate that T002113 will not be adsorbed to organic carbon in soil. T002113 is mobile. The results of the test can be considered reliable without restriction.