Registration Dossier

Data platform availability banner - registered substances factsheets

Please be aware that this old REACH registration data factsheet is no longer maintained; it remains frozen as of 19th May 2023.

The new ECHA CHEM database has been released by ECHA, and it now contains all REACH registration data. There are more details on the transition of ECHA's published data to ECHA CHEM here.

Diss Factsheets

Administrative data

Endpoint:
hydrolysis
Type of information:
experimental study
Adequacy of study:
key study
Study period:
03 September 2018 to 04 September 2018
Reliability:
2 (reliable with restrictions)

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019
Report date:
2019

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
other: Guidelines on Pecticide Residue Trials. Second Edition No. 111 Hydrolysis of a Function of pH (MEP 2013)
GLP compliance:
yes

Test material

Constituent 1
Chemical structure
Reference substance name:
(2-fluoro-3-methoxyphenyl)boronic acid
EC Number:
609-099-0
Cas Number:
352303-67-4
Molecular formula:
FC6H3(OCH3)B(OH)2
IUPAC Name:
(2-fluoro-3-methoxyphenyl)boronic acid
Test material form:
solid: particulate/powder
Specific details on test material used for the study:
Lot Number 18051400
Off White Powder
Purity 100.2%
Expiry Date 2019-03-14
Test item code 2018C021
Radiolabelling:
no

Study design

Analytical monitoring:
yes
Details on test conditions:
Preparation of Standard Solution

The stock solution of 4000 mg/L was prepared by accurately weighing 0.3997 g of the test item into a 100 mL volumetric flask. Acetontrile was added to dissolve the test item and make up to the volume. The stock solution was diluted with acetonitrile to achieve the standard solutions at concentrations of 0.5 mg/L, 1mg/L, 2 mg/L, 5 mg/L, 10mg/L, 20 mg/L, 50 mg/L and I 00 mg/L. Method linearity was evaluated by analyzing calibration standards with the method and the plot of area versus concentration. The working standard
solutions were at least 5 concentration points. The LOD of the method was 0.5 mg/L. The solution was stored in the refrigerator in E 209,P-205(2-8 °C).

The stock solution of 4000 mg/L was prepared by accurately weighing 0.40009 g of the test item into a I 00 mL volumetric flask. Acetontrile was added to dissolve the test item and make up to the volume. The stock solution was diluted with acetonitrile to achieve the standard solutions at concentrations of 200 mg/L and 20 mg/L. The fresh and old solution with the concentration of 20 mg/L was injected for 6 times and the stability was determined.

Preparation of Buffer Solution

pH4.0: 500 mL 0.1 mol/L potassium dihydrogen citrate+ 90 mL 0.1 mol/L NaOH, Water was added to make up to the volume of 1000 mL.
pH7.0: 500 mL 0.1 mol/L KH2P04 + 296.0 mL 0.1 mol/L NaOH, Water was added to make up to the volume of 1000mL.

pH9.0: 500 mL 0.1 mol/L boracic acid ( dissolved in 0.1 mol/L KC!)+ 213 mLO. l mol/L NaOH, Water was added to make up to the volume of 1000mL. All the buffer solutions used in this study were sterilized beforehand under 121 °C for 20 min.

Duration of testopen allclose all
Duration:
5 d
pH:
9
Temp.:
50 °C
Initial conc. measured:
21.08
Remarks:
Preliminary study
Duration:
5 d
pH:
7
Temp.:
50 °C
Initial conc. measured:
20.77 mg/L
Remarks:
Preliminary study
Duration:
5 d
pH:
4
Temp.:
50 °C
Initial conc. measured:
19.7 mg/L
Remarks:
Preliminary study
Number of replicates:
Preliminary test - 5
Final Test - 2
Negative controls:
not specified

Results and discussion

Preliminary study:
Preliminary Test Result (Tier I): The test item was incubated in the sterilization buffer solution with pH4.0, pH7.0 and pH9.0 at constant temperature (50±0.5 °C) in darkness for 5 days and the hydrolysis rate was 8.1 %, 29.1 % and
46.3%, respectively. The initial concentration of the test item was 19.710mg/L,

20.770mg/L and 21.008mg/L, respectively. After 5 days dark culture, the final concentration of the different buffer solutions were 18.112 mg/L, 14.726 mg/L and 11.275 mg/L. The hydrolysis rate of the test item with the pH4.0 was less than I 0%. The test item with pH4.0 sterilization buffer solution is considered
hydrolytically stable and, no additional test was required according to "The guidelines of the testing of chemicals (Second edition) No.111: Hydrolysis as a Function ofpH (SEPA, 2013) ". On the other side, the test item with pH7.0 or pH9.0 sterilization buffer solution is not stable, and had to go to the next test.

Transformation products:
not measured
Total recovery of test substance (in %)open allclose all
% Recovery:
> 94.1 - < 104.9
pH:
9
Temp.:
50 °C
Duration:
ca. 5 d
% Recovery:
> 90.6 - < 101.1
pH:
4
Temp.:
50 °C
Duration:
ca. 5 d
% Recovery:
> 94.4 - < 96.1
pH:
7
Temp.:
50 °C
Duration:
ca. 5 d
Dissipation DT50 of parent compoundopen allclose all
Key result
pH:
9
Temp.:
50 °C
DT50:
ca. 115.5
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: Hydrolytically stable based on full study of 30 days
Key result
pH:
7
Temp.:
50 °C
DT50:
115.5 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: Hydrolytically stable based on full study of 30 days
Key result
pH:
9
Temp.:
25 °C
DT50:
69.3 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: Hydrolytically stable based on full study of 30 days
Key result
pH:
7
Temp.:
25 °C
DT50:
77 d
Type:
(pseudo-)first order (= half-life)
Remarks on result:
other: Hydrolytically stable based on full study of 30 days
Details on results:
Standard solution
The following calibration samples were applied: 0.5, 1.0, 2.0, 5.0, 10.0, 20.0, 50.0 and 100 mg/L. The calibration graph was calculated applying weighted linear regression using l/concentration2 as weighting factor. The typical standard curve was: y=8.05e+004x-l.37e+003 and r=0.9993. The area deviation between old and fresh solution was 0.99% and the result indicated that the solution is stability during the study.

The following recovery samples were applied: 1 and 30 mg/L. The average recovery of test item was 10 I. I% and 90.6% and the variable coefficient was 11.3% and 2.6% with pH4 buffer solution. The average recovery of test item was 96.1 % and 94.4% and the variable coefficient was 7 .9% and I. I% with pH7 buffer solution. The average recovery of test item was I 04.9% and 94.1 % and the variable coefficient was 12.7% and 0.4% with pH9 buffer solution.

LOQ
The minimum concentration of the additive recovery was the limit of quantity (LOQ); the LOQ of FMPBA with the different buffer solutions (pH 4.0, 7 .0 and 9.0) were all 1.0 mg/L.

Preliminary Test (Tier I)

Preliminary Test Result (Tier I): The test item was incubated in the sterilization buffer solution with pH4.0, pH7.0 and pH9.0 at constant temperature (50±0.5 °C) in darkness for 5 days and the hydrolysis rate was 8.1 %, 29.1 % and 46.3%, respectively. The initial concentration of the test item was 19.710mg/L, 20.770mg/L and 21.008mg/L, respectively. After 5 days dark culture, the final concentration of the different buffer solutions were 18.112 mg/L, 14.726 mg/L and 11.275 mg/L. The hydrolysis rate of the test item with the pH4.0 was less than I 0%. The test item with pH4.0 sterilization buffer solution is considered hydrolytically stable and, no additional test was required according to "The guidelines of the testing of chemicals (Second edition) No.111: Hydrolysis as a Function ofpH (SEPA, 2013) ". On the other side, the test item with pH7.0 or pH9.0 sterilization buffer solution is not stable, and had to go to the next test.


Applicant's summary and conclusion

Validity criteria fulfilled:
not specified
Conclusions:
The FMPBA testing for hydrolysis as a function of pH was assessed according to The guidelines of the testing of chemicals (Second edition) No.111: Hydrolysis as a Function of pH ( EP, 2013 ) .
The test item was incubated in the sterilization buffer solution with pH4.0 at constant temperature (50±0.5 °C) in darkness for 5 days and the hydrolysis rate was 8.1 % which was less than 10%. The test item with pH 4.0 sterilization buffer solution is considered hydrolytically stable.
The test item was incubated in the sterilization buffer solution with pH7.0 and pH9.0 at constant temperatures (50±0.5 °C, 25±0.5 °C, 15±0.5 °C) in darkness. The result showed that the half-life (to.s) of pH7.0 at constant temperature (50±0.5 °C, 25±0.5 °C, 15±0.5 °C) was 115.5 d, 77.0 d and 10.5 d, respectively. The half-life (to.s) of pH9.0 at constant temperature (50±0.5 °C,
25±0.5 °C, 15±0.5 °C) was 115.5 d, 69.3 d, and 5.2 d.
Executive summary:

The FMPBA testing for hydrolysis as a function of pH was assessed according to the guidelines of the testing of chemicals (Second edition) No. I I I: Hydrolysis as a Function ofpH (MEP, 2013). The High Performance Liquid Chromatography  (HPLC) method was used to detect the test item.  Chromatographic  separation  was  carried  out on an Agilent Eclipse XDB-C1s Sµm (4.6IDx250  mm) column with mobile phase consisting of acetonitrile  and 0.1 % formic  acid aqueous  solution  (30/70) at a flow rate of 0.8 mL/min,  wavelength  of 210 nm. The injector volume was 20 µL.  The Average recovery  was between  90.6%-104.9%.  The minimum  detected  concentration  of the method was 1.0 mg/L. Preliminary  Test  Result (Tier   I): The  test  item  was  incubated   in   the sterilization buffer solution with pH4.0, pH7.0 and pH9.0 at constant temperature (50±0.5°C) in  darkness for 5  days and the hydrolysis rate was 8.1%,  29.1% and 46.3%, respectively.  The hydrolysis  rate of the test item with the pH4.0 was less than  I 0%.  The  test  item  with  pH4.0  sterilization  buffer  solution  is considered hydrolytically   stable  and,  no  additional  test  was  required  according  to  "The guidelines of the testing of chemicals  (Second edition) No. I I I: Hydrolysis as a Function  of pH  (MEP,  2013)   ". On the other side,  the test item with pH7.0 or pH9.0 sterilization buffer solution is not stable, and had to go to the next test.


The  test item  was incubated  in  the sterilization  buffer  solution  with pH7.0 and  pH9.0   at  constant   temperatures   (50±0.5  °C,    25±0.5  °C, 15±0.5  °C)   in darkness  for until 90% hydrolysis  was observed or for 30 days whichever  comes first.  The result  showed that the half-life (to.s) of pH7.0  at constant temperature(50±0.5  °C,   25±0.5  °C, 15±0.5  °C) was  115.5  d, 77.0 d and  10.5 d,respectively.  The  half-life  (to.s)  of  pH9.0  at  constant  temperature  (50±0.5  °C, 25±0.5 °C, 15±0.5 °C) were 115.5 d, 69.3 d, and 5.2 d.