Registration Dossier

Administrative data

Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
February 2, 2017 - February 7, 2017
Reliability:
1 (reliable without restriction)

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)
Deviations:
no
GLP compliance:
yes

Test material

Reference
Name:
Unnamed
Type:
Constituent
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Name of substance as used in the study: MTDID 15078
- Source and lot/batch No.of test material: 38022 (Drum 1)
- Purity: 95.11% sum of (3) isomers
- Expiration date of the lot/batch: May 16, 2017
Radiolabelling:
no

Study design

Analytical monitoring:
yes
Details on sampling:
-Sampling intervals for the parent/transformation products: Hydrolysis test solutions were prepared by adding approximately 500 ng of MTDID 15078 into a sterilized 20-mL amber I-Chem vial, containing 10 mL of the appropriate buffer system, for a final concentration of approximately 50 ng/mL.
- Sampling method: Two sets of triplicate samples for each pH level (total of 18 samples) was prepared. The first set of 9 samples were placed in the refrigerator on the day of preparation and as Day 0 samples. The second set of 9 samples for each pH level was placed in a cardboard box, covered with aluminum foil and placed in an orbital shaker set to 100 rpms and 50 °C for a period of (5) days (120.3 hrs.). After 5 days, the samples were prepared for analysis, along with the Day 0 samples. In addition, a method blank sample and a method spike sample were prepared for each pH level for day 0 and day 5, respectively.
- Sampling methods for the volatile compounds, if any: None
- Sampling intervals/times for pH measurements: Day 0 (prior spike with MTDID 15078) and day 5.
- Sampling intervals/times for sterility check: None
- Sample storage conditions before analysis: Day 0 samples were stored in refrigrator until day 5
- Other observation, if any (e.g.: precipitation, color change etc.): None
Buffers:
- pH: 4, 7, 9
- Type and final molarity of buffer:
pH 4: 0.1M Potassium Biphthalate + 0.1N Sodium Hydroxide;
pH 7: 0.1M Monopotassium Phosphate + 0.1N Sodium Hydroxide;
pH 9: 0.1M Boric Acid + 0.1N Sodium Hydroxide

- Composition of buffer:
pH 4 buffer: 0.4 mL 0.1N NaOH + 50 mL Biphthalate to 100 mL;
pH 7 buffer: 29.6 mL 0.1 N NaOH + 50 mL Phosphate to 100 mL;
pH 9 buffer: 21.3 mL 0.1 N NaOH + 50 mL Boric Acid to 100 mL
Details on test conditions:
TEST SYSTEM
- Type, material and volume of test flasks, other equipment used: 20-mL amber I-Chem vial
- Sterilisation method: None
- Lighting: None
- Measures taken to avoid photolytic effects: amber vial, stored in the dark
- Measures to exclude oxygen: None
- Details on test procedure for unstable compounds:
- Details of traps for volatile, if any: None
- If no traps were used, is the test system closed/open: Closed
- Is there any indication of the test material adsorbing to the walls of the test apparatus? No

TEST MEDIUM
- Volume used/treatment: 10 ML
- Kind and purity of water: Milli-Q water
- Renewal of test solution: None
- Identity and concentration of co-solvent: No co-solvent
Duration of testopen allclose all
Duration:
5 d
pH:
4
Temp.:
50 °C
Initial conc. measured:
>= 53.2 - <= 57.2 µg/L
Remarks:
average 55.5 µg/L, % RSD = 3.1
Duration:
5 d
pH:
7
Temp.:
50 °C
Initial conc. measured:
>= 50.7 - <= 57.5 µg/L
Remarks:
Average 54.3 µg/L, %RSD = 5.6
Duration:
5 d
pH:
9
Temp.:
50 °C
Initial conc. measured:
>= 56.3 - <= 61.5 µg/L
Remarks:
Average 58.5 µg/L, %RSD = 4.7
Number of replicates:
3
Positive controls:
no
Negative controls:
no

Results and discussion

Transformation products:
not measured
Dissipation DT50 of parent compound
Key result
Temp.:
25 °C
DT50:
> 1 yr
Remarks on result:
hydrolytically stable based on preliminary test
Details on results:
A Tier 1 hydrolysis of FBSEE diol was determined. The % hydrolysis at pH 4, pH 7 and pH 9 ranged from -11% to 6.3% after 5 days at 50 °C in the hydrolysis tests. Seven out of nine measurements had higher concentrations at the end of the study than the initial concentration, resulting negative values of % hydrolysis. This may be due to that the initial concentration at day 0 was not measured at day 0, rather it was stored in refrigerator and measured at day 5 with the day 5 samples .

The hydrolysis at pH 4, 7 and 9 is lower than 10% after 5 days at 50°C. As defined in OECD 111, since less than 10% of hydrolysis occurs after a period of 5 days at 50°C at pH levels of 4, 7 and 9, the test substance is considered hydrolytically stable (t 0.5 25oC > 1 year) and no further testing is required.

Any other information on results incl. tables

Table 1. Results of the hydrolysis of FBSEE diol

 

 

Day 0 concentration (ng/mL) 1

Day 5 concentration (ng/mL) 1

% hydrolysis at 50 °C

pH 4, Rep 1

53.2 (1.7)

59.2 (0.0)

-11

pH 4, Rep 2

57.2 (1.4)

59.7 (1.0)

-3.8

pH 4, Rep 3

55.1 (3.1)

57.6 (0.5)

-4.5

pH 4 Average 2

55.5 [3.8%]

58.5 [1.7%]

-6.6

pH 7, Rep 1

57.5 (1.9)

57.4 (6.3)

0.2

pH 7, Rep 2

50.7 (0.8)

54.8 (4.2)

-8.0

pH 7, Rep 3

54.6 (1.1)

55.7 (0.7)

-2.0

pH 7 Average 2

54.3 [5.6%]

56.0 [3.2%]

-3.3

pH 9, Rep 1

56.3 (1.1)

59.2 (0.0)

-5.2

pH 9, Rep 2

57.8 (7.4)

59.7 (1.0)

-3.4

pH 9, Rep 3

61.5 (0.2)

57.6 (0.5)

6.3

pH 9 Average 2

58.5 [4.7%]

58.8 [1.7%]

-0.7

 

1       Average of duplicate measurements, number in parenthesis are %RPD

2       Average of triplicate samples, number in bracket are %RSD

 

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Conclusions:
FBSEE diol has a hydrolysis half life of > 1 year under environmental conditions (25°C), it is considered hydrolytically stable.
Executive summary:

A Tier 1 hydrolysis of FBSEE diol was determined according to the OECD 111: hydrolysis as a Function of pH.

Two sets of triplicate (3) samples were prepared at a concentration of approximately 50 ng/mL of MTDID 15078 in each of pH 4, 7, and 9 buffer system, resulting in 9 hydrolysis samples for each set. The first set of 9 samples were placed in the refrigerator on the day of preparation as Day 0 samples. The second set of 9 samples were placed in a cardboard box, covered with aluminum foil and placed in an orbital shaker set to 100 rpms and 50 °C for a period of 5 days. After 5 days, the day 5 samples along with the Day 0 samples, were prepared for analysis by HPLC/MS. Hydrolysis was determined by % loss of the parent material.

The % hydrolysis at pH 4, pH 7 and pH 9 ranged from -11% to 6.3% after 5 days at 50 °C in the hydrolysis tests. As defined in OECD 111, since less than 10% of hydrolysis occurs after a period of 5 days at 50°C at pH levels of 4, 7 and 9, the test substance is considered hydrolytically stable (t 0.5 @25°C > 1 year) and no further testing is required.

This is a guideline study conducted under GLP. It is considered reliable without restriction.