Star anise, Illicium verum, ext.

Adsorption / desorption

Administrative data

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2019

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))

Version / remarks:

adopted 22. Jan. 2001

Deviations:

not specified

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))

Version / remarks:

Council Regulation (EC) No 440/2008 of 30 May 2008

Deviations:

not specified

GLP compliance:

yes (incl. QA statement)

Type of method:

HPLC estimation method

Media:

other: soil and sewage sludge

Test material

Test material information

Constituent 1

Reference substance name:

(E)-anethole

EC Number:

224-052-0

EC Name:

(E)-anethole

Cas Number:

4180-23-8

Molecular formula:

C10H12O

IUPAC Name:

1-methoxy-4-prop-1-en-1-ylbenzene

Constituent 2

Reference substance name:

4-allylanisole

EC Number:

205-427-8

EC Name:

4-allylanisole

Cas Number:

140-67-0

Molecular formula:

C10H12O

IUPAC Name:

1-allyl-4-methoxybenzene

1

Reference substance name:

Caryophyllene

EC Number:

201-746-1

EC Name:

Caryophyllene

Cas Number:

87-44-5

Molecular formula:

C15H24

IUPAC Name:

4,11,11-trimethyl-8-methylenebicyclo[7.2.0]undec-4-ene

Constituent 3

Reference substance name:

2,6-dimethyl-6-(4-methyl-3-pentenyl)bicyclo[3.1.1]hept-2-ene

EC Number:

241-702-9

EC Name:

2,6-dimethyl-6-(4-methyl-3-pentenyl)bicyclo[3.1.1]hept-2-ene

Cas Number:

17699-05-7

Molecular formula:

C15H24

IUPAC Name:

2,6-dimethyl-6-(4-methylpent-3-en-1-yl)bicyclo[3.1.1]hept-2-ene

Test material form:

liquid

Radiolabelling:

no

Study design

Test temperature:

25 ± 0.5 °C

HPLC method

Details on study design: HPLC method:

EQUIPMENT
- Apparatus: HPLC Ultimate3000
- Type, material and dimension of analytical (guard) column: moderately polar analytical columns packed with a cyanopropyl solid phase containing lipophilic and polar moieties.
-Method parameters HPLC (used for the main test)
Column: Reprosil PurCN 125*4.6 mm with pre-column Phenom-enex SecurityGuard CN, 4x3 mm
Eluent*: isocratic methanol/water 55/45 (% v/v), degassed
Flow rate: 0.8 mL/min
Injection volume: 10 µL
Column temperature: 25 ± 0.5 °C.
Wavelengh for evaluation: 220 nm (reference mix), 200 nm (test item)


MOBILE PHASES
- Type: eluent 55% methanol and 45% water, isocratic
- Experiments with additives carried out on separate columns: no
- pH: 7

DETERMINATION OF DEAD TIME
- Method: by inert substances which are not retained by the column (using an unretained compound (sodium nitrate) which was included in the mix of the reference items.)

REFERENCE SUBSTANCES
- Identity: Acetanilide (CAS#103-84-4, Batch: BCBN1982V, Purity: >= 99.0 %);
Methylbenzoate (CAS#93-58-3, Batch: BCBM9662V, Purity: >= 99.5 %);
Naphthalene (CAS#91-20-3, Batch: BCBM9272V, Purity: >= 99.7 %);
1,2,3-Trichlorobenzene (CAS#87-61-6, Batch: MKBN5959V, Purity: 99.0 %);
Phenanthrene (CAS#85-01-8, Batch: 10506, Purity: 99.5 %);
4,4’-DDT (CAS#50-29-3, Batch: SZBE057XV, Purity: 98.7 %)


REPETITIONS
- Number of determinations: 3

Results and discussion

Adsorption coefficient

Adsorption coefficient 1

Sample No.:

#1

Type:

log Koc

Value:

1.491 dimensionless

Temp.:

25 °C

Adsorption coefficient 2

Sample No.:

#2

Type:

log Koc

Value:

1.68 dimensionless

Temp.:

25 °C

Adsorption coefficient 3

Sample No.:

#3

Type:

log Koc

Value:

2.593 dimensionless

Temp.:

25 °C

Adsorption coefficient 4

Key result

Sample No.:

#4

Type:

log Koc

Value:

2.786 dimensionless

Temp.:

25 °C

Results: HPLC method

Details on results (HPLC method):

Five test item peaks were detected.
As peaks 1 – 3 and 5 showed a relative area < 5 %, they were considered as minor peaks.
Although area is not necessarily correlated to absolute concentration if a UV detector is used, it is assumed that the test item consists mainly of the peak 4. Using the correlation log k / log POW, the log KOC of the major components of the test item Essential oil of Star Anise Oil (Illicium verum) obtained from the leaves and fruits by steam distillation was calculated as 2.786 ± 0.053 (mean ± standard deviation).

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

This study was performed in order to estimate the adsorption coefficient on soil and sew-age sludge of Essential oil of Star Anise Oil (Illicium verum) obtained from the leaves and fruits by steam distillation using the HPLC-method. Using the correlation log k / log POW, the log KOC of the major components of the test item Essential oil of Star Anise Oil (Illicium verum) obtained from the leaves and fruits by steam distillation was calculated as 2.786 ± 0.053 (mean ± standard deviation).

Executive summary:

The study was performed using a HPLC with a cyanopropyl chemical bound resin on a silica basecolumn. Six reference items with different retention times were used to produce a calibration curve, since retention time on cyanopropyl columns and K_OCare correlated. The reference items were chosen on behalf of the retention time of the test itemEssential oil of Star Anise Oil (Illicium verum) obtained from the leaves and fruits by steam distillationon the column during the results of the pre-test.

A solvent blank followed by three injections of a solution of the reference items were analysed with HPLC, then three injections of a solution of the test item; and finally three injections of the solution with the reference items, in total ten runs.

For each reference item, the capacity factor k’ was calculated from the retention time of sodium nitrate and the retention time of the respective reference item. A calibration function was set up using the literature values for K_OCof the reference items and the mean capacity factor of the six determinations. In the graph log k’ versus log K_OC, linear regression was performed, giving r²= 0.9897 and r = 0.9948.

The chromatogram of the test item gave one main peak and four small peak with relative peak area > 5% each. With the calibration function log k’ versus log K_OC, the corresponding log K_OCs were determined as:

Peak	Mean Relative Peak area [%]	Mean Retention Time [min]	Log KOC+sd^1
1	0.19	2.811	1.491 ± 0.005
2	0.60	3.000	1.680 ± 0.000
3	3.39	4.242	2.593 ± 0.000
4	95.22	4.592	2.786 ± 0.000
5	0.59	22.375	> 5.63^2

¹sd = standard deviation

²Test item peak 5 lay outside the calibrated range (with log K_OC+sd6.116 ± 0.029). The log K_OCof this peak is stated as > 5.63 (log K_OCof DDT as reference item with the highest log K_OC) therefore.

These values are the means ± standard deviation of three independent determinations

Although area is not necessarily correlated to absolute concentration if a UV detector is used, it is assumed that the test item consists mainly of the peak 4. Using the correlation log k / log P_OW, the log K_OCof the major components of the test itemEssential oil of Star Anise Oil (Illicium verum) obtained from the leaves and fruits by steam distillationwas calculated as2.786±0.053 (mean ± standard deviation).