Benzonitrile, 4-formyl-3-methoxy-

Hydrolysis

Administrative data

Endpoint:

hydrolysis

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-04-23 to 2018-05-23

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:

2018

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 111 (Hydrolysis as a Function of pH)

GLP compliance:

yes (incl. QA statement)

Test material

Test material information

Constituent 1

Reference substance name:

4-formyl-3-methoxybenzonitrile

EC Number:

804-777-4

Cas Number:

21962-45-8

Molecular formula:

C9 H7 NO2

IUPAC Name:

4-formyl-3-methoxybenzonitrile

Test material form:

solid

Specific details on test material used for the study:

Name: Methoxynitrilaldehyd
CAS No.: 21962-45-8
Batch: BXR8012
Certificate of Analysis / Date: January 09, 2018
Purity: 100.5% according to CoA
Physical Appearance / Colour: White solid
Expiry Date: October 24, 2019
Storage Conditions at Test Facility: At 20°C ± 5°C in the dark

Radiolabelling:

no

Study design

Analytical monitoring:

yes

Details on sampling:

Aqueous samples were incubated and samples were taken at specific time points.
Test Duration: The incubation was terminated after 5 days.
Sampling of the Test Samples: pH 4, 7 and 9: 0, 3, 24, 120 h
At each sampling point, samples were taken in duplicate.

Buffers:

Aqueous Phase: Sterile 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 acetate buffer
410 mL CH3COOH (0.1 M) was added to 90 mL sodium acetate (0.1 M). The solution was filled up with pure water to 1 L.
pH 7: 0.05 M phosphate buffer
296 mL NaOH (0.1 M) was added to 500 mL potassium dihydrogenphosphate (0.1 M). The solution was filled up to 1 L with pure water.
pH 9: 0.05 M boric acid buffer
213 mL NaOH (0.1 M) was added to 500 mL of a solution of boric acid (0.1 M) in potassium chloride (0.1 M). The solution was filled up to 1 L with pure water.

Details on test conditions:

Test Vessels: Glass flasks (hermetically closed) were used for the test.
Test Conditions
Temperature: Preliminary test (Tier 1): 50°C ± 0.5°C
Anoxic Conditions: To avoid oxidation the buffer solutions were purged with inert gas (nitrogen) prior to sterilisation.
Sterile Conditions: Degased buffer solutions and the used glassware were sterilised using an autoclave (20 min at 121°C) prior to application. Aqueous solution buffered at pH 4 was sterilized by filtration
Application
Stock/Application Solutions
Stock Solution of the Test Item: Two individual stock solutions (A and B) were prepared in acetonitrile (ACN) with a concentration of 5.0 and 5.2 g/L.
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). Therefore 0.499 mL of the stock solution A and 0.478 mL of the stock solution B were pipetted to 50 mL of each buffer solution resulting in a nominal concentration of approximately 50 mg/L.
Number of Samples: 8 samples per pH level
Preparation of the Blank Samples
Blank Samples: A blank sample for each pH was prepared which consisted of the buffer solution (without application of the test item).
Number of Samples: 1 sample per pH level
Test Parameters
Temperature: The temperature was recorded continuously.
pH-Value: The pH of the sample solution was determined at each sampling point.
Sterility of the Test Solution: A sterility confirmation test was carried out during the preliminary test. A commercially available dip slide kit (TSA with TTC and Rose Bengal Chloramphenicol Agar, VWR Chemicals) was used for a total count of microorganisms and to determine the total count of yeast and moulds.

Duration of test

Duration of test 1

Duration:

0 h

pH:

4

Temp.:

50 °C

Initial conc. measured:

49.55 mg/L

Duration of test 2

Duration:

0 h

pH:

7

Temp.:

50 °C

Initial conc. measured:

48.8 mg/L

Duration of test 3

Duration:

0 h

pH:

9

Temp.:

50 °C

Initial conc. measured:

49.25 mg/L

Number of replicates:

At each sampling point and for each pH level samples were taken in duplicate.

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 91-99% of the nominal concentration. Thus the test item can be stated as hydrolytically stable. The main test (Tier 2) was not performed.

Test performance:

According to the preliminary study Methoxynitrilaldehyd can be stated as hydrolytically stable. The main test (Tier 2) was not performed.

Transformation products:

no

Total recovery of test substance (in %)

Total recovery of test substance (in %) 1

% Recovery:

99

St. dev.:

2.7

pH:

4

Temp.:

50 °C

Duration:

120 h

Remarks on result:

hydrolytically stable based on preliminary test

Total recovery of test substance (in %) 2

% Recovery:

99.1

St. dev.:

1.3

pH:

7

Temp.:

50 °C

Duration:

120 h

Remarks on result:

hydrolytically stable based on preliminary test

Total recovery of test substance (in %) 3

% Recovery:

90.7

St. dev.:

0.7

pH:

9

Temp.:

50 °C

Duration:

120 h

Remarks on result:

hydrolytically stable based on preliminary test

Dissipation DT50 of parent compound

Remarks on result:

hydrolytically stable based on preliminary test

Details on results:

The present study investigated the hydrolytic behaviour of Methoxynitrilaldehyd 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, 91-99% of the nominal concentration were found and thus the test item can be stated as hydrolytically stable (t0.5 > 1 year at 25°C).

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Remarks:

Immediately after application (0 h) recoveries of the samples of pH 4, 7 and 9 were in the range of 97-101% of the nominal concentration.

Conclusions:

The present study investigated the hydrolytic behaviour of Methoxynitrilaldehyd 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, 91-99% of the nominal concentration were found and thus the test item can be stated as hydrolytically stable (t0.5 > 1 year at 25°C).

Executive summary:

Title: Methoxynitrilaldehyd: Hydrolysis as a Function of pH [OECD 111]

Test Item: Methoxynitrilaldehyd

Guidelines/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 Methoxynitrilaldehyd at different environmentally relevant pH-values and at different temperatures.

Test Setup: Test Vessels: Glass flasks were used for the test.

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

Test Conditions: In the dark at 50°C ± 0.5°C (Preliminary test (Tier 1))

Treatment Rate: 50 mg/L (two individual replicates)

Results:               

The present study investigated the hydrolytic behaviour of Methoxynitrilaldehyd 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, 91-99% of the nominal 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.