Glycerides, tall-oil mono-

Partition coefficient

Link to relevant study record(s)

Reference

Endpoint:

partition coefficient

Type of information:

experimental study

Adequacy of study:

key study

Study period:

17. Aug. 2018 to 24. Aug. 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 117 (Partition Coefficient (n-octanol / water), HPLC Method)

Version / remarks:

OECD Guidelines for the Testing of Chemicals, Method No. 117, adopted 13. April 2004: “Partition Coefficient (n-octanol/water), High Performance Liquid Chromatography (HPLC) Method“.

Deviations:

yes

Remarks:

See "Any other information" for details

Qualifier:

according to guideline

Guideline:

other: EC No. 440/2008, Method A.24

Version / remarks:

Commission Regulation (EU) 2016/266 adopted 7 December 2015 amending Regulation EC No. 440/2008, Method A.24 “Partition Coefficient (N-OCTANOL/WATER), HIGH PERFORMANCELIQUID CHROMATOGRAPHY (HPLC) METHOD

Deviations:

yes

Remarks:

See "Any other information" for details

GLP compliance:

yes (incl. QA statement)

Type of method:

HPLC method

Partition coefficient type:

octanol-water

Specific details on test material used for the study:

No further details specified in the study report.

Analytical method:

high-performance liquid chromatography

Key result

Type:

log Pow

Partition coefficient:

> 4.761 - <= 6.5

Temp.:

25 °C

Remarks on result:

other: pH not specified in the study report

Details on results:

Result
Using the correlation log k / log POW, the log POW of peak 1 of the test item
LUMULSE GMT-K was calculated as 4.761 ± 0.001 (mean ± standard deviation). The log POW of test item peak 2 was extrapolated with 6.551 ± 0.002. For test item peaks 3 – 7 no calculations could be performed, because these peaks eluted in the not isocratic part of the HPLC program. Because the retention time of the test item peaks 3 - 7 is higher than the retention time of DDT (27.1 min.), the log POW of these peaks is stated as > 6.5 (log POW of DDT as reference with the highest log POW).
The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5.

DISCUSSION
Variations in the retention times of reference items and test item were very small, demonstrating a sta-ble configuration of the HPLC-column.
The correlation log k / log POW is good: the coefficient of determination r2 was calculated with 0.995. This value was considered as sufficiently high to use the calibration function for the determination of the log POW of the test item LUMULSE GMT-K.
A test item solution, prepared in methanol, showed seven signals. Only one test item peak lay in the cali-brated range. Peak 1 has a log POW of 4.761 ± 0.001 (mean ± standard deviation). Peak 2 eluted in the iso-cratic part of the program too but outside the calibrated range. The log POW of test item peak 2 was ex-trapolated with 6.551 ± 0.002.
Five peaks eluted in the not isocratic part of the HPLC program after the retention time of DDT and change of the mobile phase to 100 % methanol. The mobile phase was changed to 100 % methanol to show, that the test item contains ingredients, which are detectable and elute from the HPLC column after DDT. The log POW of these test item peaks are stated as > 6.5 (log POW of DDT).
The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5 therefore.
No observations were made which might cause doubts concerning the validity of the study outcome.

Findings and Results

Reference Items

Measurement Data

The retention times which were recorded for the reference items are presented in the following table.

Retention Times (RT) Reference Items and dead time marker

Compound	RT 1	RT 2	RT 3	RT 4	RT 5
	min.	min.	min.	min.	min.
Thiourea	1.393	1.393	1.397	1.393	1.393
2-Butanone	1.707	1.707	1.710	1.707	1.710
Acetophenone	2.110	2.113	2.117	2.113	2.117
Naphthalene	4.780	4.790	4.793	4.787	4.797
Diphenyl ether	6.220	6.230	6.237	6.233	6.247
Phenanthrene	8.700	8.717	8.727	8.720	8.740
Fluoranthene	11.873	11.897	11.913	11.910	11.937
Triphenylamine	20.133	20.163	20.200	20.200	20.243
DDT	27.073	27.087	27.127	27.163	27.213

 

Calculated Values

For each reference item, the calculated capacity factors are presented in the following table.

Capacity factors Reference Items and dead time marker

Compound	Retention Time Mean	Retention Time Standard  Deviation	Retention Time Relative Standard Deviation	k
	min.	min.	%
Thiourea	1.394	0.001	0.107	0.0000
2-Butanone	1.708	0.002	0.107	0.2253
Acetophenone	2.114	0.003	0.132	0.5165
Naphthalene	4.789	0.006	0.134	2.4357
Diphenyl ether	6.233	0.010	0.156	3.4715
Phenanthrene	8.721	0.015	0.167	5.2559
Fluoranthene	11.906	0.023	0.195	7.5409
Triphenylamine	20.188	0.042	0.206	13.4821
DDT	27.133	0.057	0.211	18.4639

 

log POW / log k

The values for log k and log POW of the reference items are presented in the following table:

log k and log POW of Reference Items

Compound	log k	log POW
2-Butanone	-0.6473	0.3
Acetophenone	-0.2869	1.7
Naphthalene	0.3866	3.6
Diphenyl ether	0.5405	4.2
Phenanthrene	0.7206	4.5
Fluoranthene	0.8774	5.1
Triphenylamine	1.1298	5.7
DDT	1.2663	6.5

 

Test Item LUMULSE GMT-K

Measurement Data

The retention times and areas of the test item peaks are presented in the following tables:

Retention Times (RT) Test Item

Measurement	RT 1	RT 2	RT 3	RT 4
	min.	min.	min.	min.
Measurement 1	9.4300	31.8500	38.5967	38.7567
Measurement 2	9.4167	31.7733	38.5900	38.7500
Measurement 3	9.4233	31.8400	38.5933	38.7533
Mean	9.423	31.821	38.593	38.753
Standard Deviation	0.007	0.042	0.003	0.003
Measurement	RT 5	RT 6	RT 7
	min.	min.	min.
Measurement 1	39.2400	44.2833	45.4167
Measurement 2	39.2267	44.2933	45.3867
Measurement 3	39.2300	44.2767	45.3767
Mean	39.232	44.284	45.393
Standard Deviation	0.007	0.008	0.021

 

Peak Areas Test Item

Measurement	Area Peak 1	Relative Area Peak 1	Area Peak 2	Relative Area Peak 2*
	mAU*min	%	mAU*min	%
Measurement 1	2.9018	9.28	0.9988	3.19
Measurement 2	2.8641	9.28	0.9974	3.23
Measurement 3	2.9377	9.70	0.8086	2.67
Mean	2.901	9.42	0.935	3.03
Relative Standard Deviation	1.27 %	2.61 %	11.70 %	10.32 %
Measurement	Area Peak 3	Relative Area Peak 3	Area Peak 4	Relative Area Peak 4*
	mAU*min	%	mAU*min	%
Measurement 1	8.8851	28.41	1.0270	3.28
Measurement 2	8.9108	28.86	1.1366	3.68
Measurement 3	8.7599	28.94	1.0944	3.62
Mean	8.852	28.74	1.086	3.53
Relative Standard Deviation	0.91 %	0.99 %	5.09 %	6.04 %
Measurement	Area Peak 5	Relative Area Peak 5	Area Peak 6	Relative Area Peak 6
	mAU*min	%	mAU*min	%
Measurement 1	2.7501	8.79	3.5030	11.20
Measurement 2	2.5449	8.24	2.7340	8.85
Measurement 3	2.4577	8.12	2.7852	9.20
Mean	2.584	8.39	3.007	9.75
Relative Standard Deviation	5.81 %	4.29 %	14.30 %	12.99 %
Measurement	Area Peak 7	Relative Area Peak 7
	mAU*min	%
Measurement 1	11.2064	35.83
Measurement 2	11.6877	37.85
Measurement 3	11.4296	37.75
Mean	11.441	37.15
Relative Standard Deviation	2.11 %	3.06 %

 

Calculated Values

The calculated values are presented in the following table:

Capacity Factor, log Capacity Factor, log P_OWTest Item Peaks 1 and 2

Peak	Measurement No.	k	log k	log POW
1	1	5.7647	0.7608	4.762
	2	5.7551	0.7601	4.760
	3	5.7599	0.7604	4.761
	Mean			4.761
	Standard Deviation			0.001
2*	1	21.8479	1.3394	6.552
	2	21.7929	1.3383	6.548
	3	21.8407	1.3393	6.551
	Mean			6.551
	Standard Deviation			0.002

*The result of test item peak 2 lay outside the calibrated range of the reference items (log P_OWof DDT as reference with the highest log P_OW is 6.5). The log P_OW, stated in this table, is obtained by extrapolation therefore.

 

The log P_OWwas calculated from the capacity factors as follows:

log P_OW= (log k + 0.7784) / 0.3232

Conclusions:

The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5.

Executive summary:

Determination of the log POW of LUMULSE GMT-K using the HPLC method according to OECD 117 resp. EU A.24

 

Findings:         

The study was performed using an HPLC with a C18 column. Eight reference items with different retention times and thiourea for the determination of the dead time were used to produce a calibration curve, since retention time on hydrophobic columns and POW are correlated. The reference items were chosen based on the results of the pre-test.

 

A test item solution in methanol showed signals with UV detection before and after the retention time of DDT and also after the change of the mobile phase to 100 % methanol. The mobile phase methanol/water 75/25 % (v/v) was changed after 35 minutes to 100 % methanol to show, that the test item contains ingredients, which are detectable and elute from the HPLC column after DDT.

 

One vial was filled with the reference item mix and one vial with the test item solution. The vials were analysed using the HPLC with the program described below. First one injection from the solvent blank methanol was made. Then three injections were measured from the reference item mix, three injections from the test item and two injections from the reference item mix.

 

For each reference item, the capacity factor k was calculated from the retention time of thiourea and the retention time of the respective reference item.

 

A calibration function (log k versus log POW, linear fit) was determined using the literature values for POW of the reference items and the retention times in the five determinations.

 

The test item solution, prepared in methanol, showed seven signals. Only test item peak 1 lay in the calibrated range. With the calibration function log k versus log POW, the corresponding log POW of peak 1 was determined with: 4.761 ± 0.001 (mean ± standard deviation).

 

Peak 2 eluted in the isocratic part of the program too but outside the calibrated range. The log POW of test item peak 2 was extrapolated with 6.551 ± 0.002.

 

Five peaks eluted in the not isocratic part of the HPLC program after the retention time of DDT and change of the mobile phase to 100 % methanol. The log POW of these test item peaks are stated as > 6.5 (log POW of DDT).

 

The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5.

Description of key information

The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5.

Key value for chemical safety assessment

Log Kow (Log Pow):

6.5

at the temperature of:

25 °C

Additional information

The study was performed using an HPLC with a C18 column.

The test item solution, prepared in methanol, showed seven signals. Only test item peak 1 lay in the calibrated range. With the calibration function log k versus log POW, the corresponding log POW of peak 1 was determined with: 4.761 ± 0.001 (mean ± standard deviation).

Peak 2 eluted in the isocratic part of the program too but outside the calibrated range. The log POW of test item peak 2 was extrapolated with 6.551 ± 0.002.

Five peaks eluted in the not isocratic part of the HPLC program after the retention time of DDT and change of the mobile phase to 100 % methanol. The log POW of these test item peaks are stated as > 6.5 (log POW of DDT).

The log POW of test item LUMULSE GMT-K is stated as range 4.761 to > 6.5.