Registration Dossier

Administrative data

Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
30/01/2017 to 04/04/2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report Date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
OECD Guideline 105 (Water Solubility)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.6 (Water Solubility)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
column elution method

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Details on test material:
- Appearance: solid yellow powder

Results and discussion

Water solubility
Key result
Water solubility:
0.483 mg/L
Conc. based on:
test mat.
Temp.:
20 °C
pH:
4.5

Any other information on results incl. tables

Preliminary test result:

Test Item

[mg]

total volume of ultra-pure water
[mL]

time of shaking

[min]

remarks

Approximate solubility

[mg/L]

 

100

10

not completely dissolved

< 101

10.1

200

10

 not completely dissolved

< 50.5

 

300

10

 not completely dissolved

< 33.7

 

400

10

 not completely dissolved

< 25.3

 

500

10

 not completely dissolved

< 20.2

 

1000

10

 not completely dissolved

< 10.1

 

1000

17 hours

 not completely dissolved

< 10.1

 

1100

74 hours

not completely dissolved

< 9.2

The minimum amount of test item needed for the main test is: 5 x 9.2 mg/L = 46 mg/L = 2.3 mg/50 mL

Main test:

Amount of test item in each column: ≥ 2.5 mg at 50 mLwater

sampling time

Analyte concentration column 1 (25 mL/h)

Analyte concentration column 2 (8 mL/h)

pH value
column 1

pH value
column 2

[h]

[mg/L]

[mg/L]

 

 

405

0.512

0.598

4.5

4.5

429

0.338

0.373

4.5

4.5

453

0.461

0.513

4.5

4.5

479

0.424

0.577

4.5

4.5

501

0.478

0.551

4.5

4.5

Mean:*

0.443

0.522

4.5

4.5

SD:*

0.067

0.089

0.0

0.0

RSD [%]:*

15.1

17.0

0.0

0.0

 

Analyte concentration [mg/L]

pH Value

Overall mean:*

0.483

4.5

Overall AD:*

0.079

0.0

Overall RD [%]:*

16.4

0.0

SD: standard deviation; RSD: relative standard deviation; AD: absolute deviation; RD: relative deviation

* : values were calculated from the last 5 consecutive samples

 

The results indicate the required reproducibility (relative standard deviation below 30 %) and no tendency to increasing values, when the test time is prolonged.

The mean values obtained from the two tests with different flows did not differ by more than 30 %.

The analytical method used was validated. The calibration curve was linear with R= 1. The LOQ was set at 0.2318 mg/L and LOD at 0.1 mg/L. The recovery was found to be 98.6 % and 99.9 % for 0.2318 and 1.714 mg/L respectively.

Applicant's summary and conclusion

Conclusions:
The water solubility was determined to be 0.483 mg/L (20°C, pH 4.5).
Executive summary:

In the current study the water solubility of the test item was determinde according to OECD guideline 105 (1995) and Council Regulation (EC) No. 440/2008 Method A.6. The study was according to GLP. The solubility of the test item was determined using the column elution method at 20 +/- 0.5°C.

The HPLC method (HPLC with UV detection ) for the determination of the content of Mordant Red 11 in aquaeous solutions was validated and tested with satisfactory results in regard to linearity of the detector, accuracy, precision and non-analyte interference of the analytical system.

The water solubility was determined to be 0.483 mg/L (20°C, pH 4.5).