Registration Dossier

Administrative data

Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
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 guideline
Qualifier:
according to
Guideline:
OECD Guideline 111 (Hydrolysis as a Function of pH)
GLP compliance:
yes (incl. certificate)

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
other: solution of the substance in water
Radiolabelling:
no

Study design

Analytical monitoring:
yes
Details on sampling:
Test System
Aqueous Phase: Aqueous solutions buffered at pH 4, 7 and 9.
The pH of each buffer solution was measured with a calibrated pH meter.
pH 4: 0.05 M phthalate buffer
500 mL of 0.1 M potassium hydrogen phthalate solution (10.215 g/500 mL pure water) was mixed with 40 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
pH 7: 0.05 M phosphate buffer
500 mL potassium dihydrogen phosphate solution (6.804 g/500 mL pure water) was mixed with 296 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
pH 9: 0.05 M boric acid buffer
500 mL boric acid solution (3.091 g/500 mL 0.1 M KCl solution) was mixed with 213 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
Test Units
Test Vessels: Glass flasks were used for the test.
Test Conditions
Temperature: 50°C ± 0.1°C
Anoxic Conditions: To avoid oxidation the buffer solutions were purged with inert gas (nitrogen) prior to sterilisation.
Sterile Conditions: The buffer solutions were sterile filtered (0.2 µm).
The used glassware was sterilised using an autoclave (20 min at 121°C) prior to application.
Application
Stock/Application Solutions
Stock Solution of the Test Item: The stock solutions were prepared in sterile pure water with a concentration of 1000.2 mg/L and 1000.6 mg/L, respectively.
Application Solution of the Test Item: The stock solutions were used.
Application of the Test Samples
The final concentration of the test item in the aqueous phase was below 0.01 M or half of its water solubility and the content of organic was < 1% v/v.
Application Procedure: Test sample solutions were prepared in duplicate (A and B). Hereto 0.5 mL of the stock solutions (A and B) was separately pipetted to 50 mL of each buffer solution resulting in a nominal concentration of 10 mg/L.
Aliquots of the test solutions were transferred to the test vessels.
Number of Samples: 8 samples per pH level
Course of the Study
Aqueous samples were incubated and duplicate samples were taken at specific time points.
Preliminary Test (Tier 1)
Test Duration: The test was executed for 5 days.
Sampling of the Test Samples: pH 4, 7 and 9: 0 and 120 h
Test Parameters
pH-Value: The pH-value was determined at each sampling point.
Temperature: The temperature was recorded continuously.
Sterility of the Test Solution: A sterility confirmation test was carried out during the preliminary test. A commercially available dip slide kit (Hycon GK-T/HS, Heipha Dr. Müller GmbH, Eppelheim, Germany) was used for a total count of microorganisms and to determine the total count of yeast and moulds.
Buffers:
Aqueous solutions buffered at pH 4, 7 and 9.
The pH of each buffer solution was measured with a calibrated pH meter.
pH 4: 0.05 M phthalate buffer
500 mL of 0.1 M potassium hydrogen phthalate solution (10.215 g/500 mL pure water) was mixed with 40 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
pH 7: 0.05 M phosphate buffer
500 mL potassium dihydrogen phosphate solution (6.804 g/500 mL pure water) was mixed with 296 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
pH 9: 0.05 M boric acid buffer
500 mL boric acid solution (3.091 g/500 mL 0.1 M KCl solution) was mixed with 213 mL of 0.1 M sodium hydroxide solution and was adjusted to a final volume of 1000 mL using pure water.
Details on test conditions:
Temperature: 50°C ± 0.1°C
Anoxic Conditions: To avoid oxidation the buffer solutions were purged with inert gas (nitrogen) prior to sterilisation.
Sterile Conditions: The buffer solutions were sterile filtered (0.2 µm).
The used glassware was sterilised using an autoclave (20 min at 121°C) prior to application.
Duration of testopen allclose all
Duration:
5 d
pH:
4
Temp.:
50 °C
Initial conc. measured:
10 mg/L
Duration:
5 d
pH:
7
Temp.:
50 °C
Initial conc. measured:
10 mg/L
Duration:
5 d
pH:
9
Temp.:
50 °C
Initial conc. measured:
10 mg/L
Number of replicates:
Two samples of solutions of each pH value at each test temperature were taken at each sampling point.
Positive controls:
no
Negative controls:
no

Results and discussion

Preliminary study:
Samples were incubated at three different pH-values and at one temperature. The test was carried out for 5 days. During incubation the concentration of the test item remained stable at each tested pH-value of 4, 7 and 9. Recoveries (mean) were in the range of 97.5-102.7% of the nominal applied concentration. After 5 days of incubation, 97.5-98.4% of the nominal applied concentration was found and thus the test item can be stated as hydrolytically stable. Tier 2 was not performed.
Test performance:
Samples, in a nominal concentration of 10 mg/L, were incubated at three different pH-values and at one temperature. The test was carried out for 5 days.
Transformation products:
not measured
Total recovery of test substance (in %)open allclose all
% Recovery:
97.5
pH:
4
Temp.:
50 °C
Duration:
5 d
% Recovery:
98.4
pH:
7
Temp.:
50 °C
Duration:
5 d
% Recovery:
97.7
pH:
9
Temp.:
50 °C
Duration:
5 d
Dissipation DT50 of parent compoundopen allclose all
pH:
4
Temp.:
25 °C
DT50:
> 1 yr
pH:
7
Temp.:
25 °C
DT50:
> 1 yr
pH:
9
Temp.:
25 °C
DT50:
> 1 yr

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Remarks:
Accuracy of the Applied Concentration: Immediately after application (0 h) recoveries of the samples of pH 4, 7 and 9 were in the range of 98.1-103.5% of the nominal applied concentration.
Conclusions:
The present study investigated the hydrolytic behaviour of the test itemin aqueous solutions buffered at pH 4, 7 and 9 and at one elevated temperature. Samples were incubated in the dark. The test was carried out for 5 days. At the end of incubation, 97.5-98.4% of the nominal applied concentration were found and thus the test item can be stated as hydrolytically stable (t0.5 > 1 year at 25°C).
Executive summary:

Title:     Sanolin Lave Blue A VP 5453: Hydrolysis as a Function of pH [OECD 111]

Test Item: Sanolin Lave Blue A VP 5453

Guidelines/Recommendations: This study was based on the procedures indicated by the following internationally accepted guidelines and recommendations: OECD Guideline for Testing of Chemicals No. 111: "Hydrolysis as a function of pH", adopted April 13, 2004.

GLP: Yes (certified laboratory)

Purpose: The purpose of the study was to determine the rate of hydrolysis of Sanolin Lave Blue A VP 5453 at different environmentally relevant pH-values and at different temperatures.

Test Setup: Test Vessels:

Test vessels used for the test were made of glass.

Aqueous Solution: Aqueous solutions buffered at pH 4, 7 and 9.

Test Conditions: 50°C ± 0.1°C, in the dark

Treatment Rate: 10 mg/L (two individual replicates)

Results:

The present study investigated the hydrolytic behaviour of Sanolin Lave Blue A VP 5453 in aqueous solutions buffered at pH 4, 7 and 9 and at one elevated temperature. Samples were incubated in the dark. The test was carried out for 5 days. At the end of incubation, 97.5-98.4% of the nominal applied concentration were found and thus the test item can be stated as hydrolytically stable (t0.5 > 1 year at 25°C).

This study is classified acceptable and satisfies the guideline requirements for hydrolysis studies.