2-[[3-acetamido-4-[(2-chloro-4-nitrophenyl)azo]phenyl](2-cyanoethyl)amino]ethyl acetate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From May 22th to June 6th, 2019

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

2008

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

1995

GLP compliance:

yes (incl. QA statement)

Type of method:

column elution method

Water solubility:

< 1.08 mg/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

6.98

Details on results:

-Preliminary test: the preliminary test at room temperature showed that the water solubility of the test item was below 4.39 mg/l. Therefore the column elution method was performed.
-Main test: the mean value and its standard deviation from five consecutive samples taken from the saturation plateau, each measured twice, were calculated for each run. The mean concentrations calculated on two test using different flows were compared and the repeatability was calculated, which should be better than 30 %. As no signal of the test item could be detected in the fractions, the first column showed a value of the water solubility of <1.08 mg/l (To verify the accuracy of the analytical method freshly prepared standard solutions (prepared with the test item) were measured in between the samples of the column elution method. The recovery rates should liebetween 90 and 110 %. The recovery rate of the measured standard solutions was in the range from 96.1 % to 102.7 %, which shows a good accuracy of
the analytical method.
Following the measurements, the amount of the test item in the columns was checked. For this purpose, columns 1 and 2 were each purged with 100 ml acetone. 0.05 ml of the acetone solutions were diluted to 1 ml with the eluent and measured by HPLC.
These measurements show, that 9.90 mg of the test item could be found in column 1 after the main test, which corresponds to 47.5 % of the starting amount. 10.60 mg of the test item could be found in column 2 after the main test, which corresponds to 50.9 % of the starting amount. In both columns enough test item could be found after the main tests to ensure correct performance of the test.

Measurement of standard solutions

Standard solution	Measured value [mg/l]	Recovery rate [ % ]
(nominal value [mg/l])
Standard-Ü1 (1.368)	1.349	98.6
	1.373	100.4
	1.365	99.8
Standard-Ü2 (3.218)	3.204	99.6
	3.224	100.2
	3.125	97.1
Standard-Ü3 (4.416)	4.36	98.7
	4.537	102.7
Standard-Ü4 (5.066)	5.04	99.5
	4.868	96.1

Summarised results of column 1 and 2

Column	Mean concentration	Mean measured concentration	Relative standard deviation (RSD)
	[mg/l]	[mg/l]	[ % ]
1	< 1.08	< 1.08	--
2	< 1.08

Conclusions:

According to OECD Test Guideline 105 (1995) the water solubility at 20°C of the test item was estimated to be below the LOD: cs < 1.08 mg/l.

Executive summary:

The mean value and its standard deviation from five consecutive samples taken from the saturation plateau, each measured twice, were calculated for each run. The mean concentrations calculated on two tests using different flows were compared and the repeatability was calculated, which should be better than 30 %.  

As no signal of the test item could be detected in the fractions, first, second and third columns showed a value of the water solubility of <1.08 mg/l (<LOD).

To verify the accuracy of the analytical metho,d freshly prepared standard solutions were measured in between the samples of the column elution method. The recovery rates should lie between 90 and 110 %. The recovery rate of the measured standard solutions was in the range from 96.1 % to 102.7 %, which shows a good accuracy of the analytical method.

Overall, the water solubility at 20 °C of the test item was estimated to be below the LOD, i.e. < 1.08 mg/l.

Description of key information

Water solubility at 20 °C was estimated to be below the LOD: c_S < 1.08 mg/l.

Key value for chemical safety assessment

at the temperature of:

20 °C

Additional information

OECD guideline 105 (1995).