Registration Dossier

Physical & Chemical properties

Solubility in organic solvents / fat solubility

Administrative data

Endpoint:
solubility in organic solvents / fat solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 18-Oct-2010 to 22-Oct-2010
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: This study has been performed according to OJEC and CIPAC guidelines and according to GLP principles.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2010
Report date:
2010

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
other: CIPAC MT 181
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: OJEC A.6
Deviations:
no
GLP compliance:
yes (incl. QA statement)

Test material

Constituent 1
Chemical structure
Reference substance name:
Ascophyllum nodosum, ext.
EC Number:
283-907-6
EC Name:
Ascophyllum nodosum, ext.
Cas Number:
84775-78-0
Molecular formula:
Not applicable; a generic molecular formula cannot be provided for this UVCB substance.
IUPAC Name:
(2R,3R,4R,5R)-hexane-1,2,3,4,5,6-hexol; (2S,3S,4S,5S,6R)-6-{[(2S,3S,4R,5S,6R)-2-carboxy-4,5,6-trihydroxyoxan-3-yl]oxy}-3,4,5-trihydroxyoxane-2-carboxylic acid; [(2S,3R,4R,5S,6S)-3-hydroxy-6-{[(2S,3R,4R,5S,6S)-3-hydroxy-6-{[(2S,3R,4R,5S,6S)-6-{[(2S,3R,4R,5S,6S)-3-hydroxy-6-{[(2S,3R,4R,5S,6R)-6-hydroxy-2-methyl-4,5-bis(sulfooxy)oxan-3-yl]oxy}-2-methyl-5-(sulfooxy)oxan-4-yl]oxy}-2-methyl-4,5-bis(sulfooxy)oxan-3-yl]oxy}-2-methyl-5-(sulfooxy)oxan-4-yl]oxy}-2-methyl-5-(sulfooxy)oxan-4-yl]oxidanesulfonic acid
Details on test material:
Test item identification : Algea Fert Solid K+
Empirical formula : not available
Structural formula : not available
Molecular weight : Not available
Batch number : 00680
ChemService number : 2901493-001
Manufacturing date : March 09, 2010
Expiry date : March 09, 2012

Results and discussion

Solubility in organic solvents / fat solubilityopen allclose all
Medium:
methanol
Solubility:
250.6 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Medium:
other: dichloromethane
Solubility:
9.9 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Medium:
other: n-hexane
Solubility:
< 1 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Medium:
other: p-xilene
Solubility:
1.4 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Medium:
acetone
Solubility:
7 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Medium:
ethyl acetate
Solubility:
9 mg/L
Temp.:
22 °C
Remarks on result:
other: with analytical determination with OJEC A.6 method
Test substance stable:
yes

Any other information on results incl. tables

Method CIPAC MT 181

No solubility data were found in literature.

Since in the preliminary test, a test item solubility in every solvent tested lower than 10 g/L was estimated, an analytical determination was performed using the shake flask method described in OJEC Method A.6, with the aim to obtain a more accurate value.

 

 

Shake flask method (OJEC A.6)

  

The results of the solvent solubility test are reported in Tables from 4 to 11.

The quality criteria of the Method A.6 were verified (RSD% over three values is < 15%).

 

Representative spectra are presented in Figures from 1 to 6.

 

TABLE 1 Linear calibration for Methanol

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 275 nm

0.0122

0.1014

0.8653

2nd series 275 nm

0.0135

0.1017

0.8478

Mean

0.0129

0.1016

0.8565

Delta

0.0013

0.0004

0.0175

Delta %

10.00%

0.35%

2.05%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0080

0.0104

0.99991

 

TABLE 2 Results obtained for Methanol solubility

 

ChemService

code

As – Ab

275 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

0.0000

-

-

-

-

-

2901493-001 MeOH A1

0.5158

62.80

4.00

1.00

251.18

251.07

2901493-001 MeOH A2

0.5153

62.74

4.00

1.00

250.95

2901493-001 MeOH B1

0.5150

62.69

4.00

1.00

250.76

250.60

2901493-001 MeOH B2

0.5143

62.61

4.00

1.00

250.43

2901493-001 MeOH C1

0.5135

62.51

4.00

1.00

250.05

250.02

2901493-001 MeOH C2

0.5134

62.50

4.00

1.00

249.99

Mean value :

250.6

Standard deviation (S.D.) :

0.49

Relative Standard Deviation (RSD%):

0.19%

 

(1) Quantification with the linear calibration curve.


 

TABLE 3 Linear calibration for Dichloromethane

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 275 nm

0.0217

0.0981

0.8635

2nd series 275 nm

0.0211

0.0980

0.8654

Mean

0.0214

0.0981

0.8644

Delta

0.0007

0.0001

0.0019

Delta %

3.22%

0.10%

0.22%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0081

0.0129

1.00000

 

TABLE 4 Results obtained for Dichloromethane solubility

 

ChemService

code

As – Ab

275 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

-0.0001

-

-

-

-

-

2901493-001 DCM A1

0.0952

10.17

1.00

1.00

10.17

10.29

2901493-001 DCM A2

0.0972

10.41

1.00

1.00

10.41

2901493-001 DCM B1

0.0921

9.79

1.00

1.00

9.79

9.69

2901493-001 DCM B2

0.0906

9.60

1.00

1.00

9.60

2901493-001 DCM C1

0.0875

9.22

1.00

1.00

9.22

9.58

2901493-001 DCM C2

0.0934

9.95

1.00

1.00

9.95

Mean value :

9.9

Standard deviation (S.D.) :

0.42

Relative Standard Deviation (RSD%):

4.29%

 

(1) Quantification with the linear calibration curve.


 

TABLE 5 Linear calibration for n-Hexane

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 275 nm

0.0256

0.0980

0.8654

2nd series 275 nm

0.0217

0.1039

0.8584

Mean

0.0237

0.1009

0.8619

Delta

0.0038

0.0058

0.0070

Delta %

16.21%

5.79%

0.81%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0080

0.0157

1.00000

 

TABLE 6 Results obtained for n-Hexane solubility

 

ChemService

code

As – Ab

275 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

0.0004

-

-

-

-

-

2901493-001 n-Hexane A1

0.0068

0.30

1.00

1.00

0.30

0.26

2901493-001 n-Hexane A2

0.0047

0.21

1.00

1.00

0.21

2901493-001 n-Hexane B1

0.0036

0.16

1.00

1.00

0.16

0.15

2901493-001 n-Hexane B2

0.0033

0.15

1.00

1.00

0.15

2901493-001 n-Hexane C1

0.0024

0.11

1.00

1.00

0.11

0.10

2901493-001 n-Hexane C2

0.0022

0.10

1.00

1.00

0.10

Mean value :

0.2

Standard deviation (S.D.) :

-

Relative Standard Deviation (RSD%):

-

 

(1) Quantification with the lowest standard calibration curve (WSS 1).


 

TABLE 7 Linear calibration for p-Xylene

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 300 nm

0.0149

0.0839

0.6927

2nd series 300 nm

0.0171

0.0833

0.6972

Mean

0.0160

0.0836

0.6949

Delta

0.0021

0.0006

0.0046

Delta %

13.29%

0.67%

0.66%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0065

0.0121

0.99997

 

TABLE 8 Results obtained for p-Xylene solubility

 

ChemService

code

As – Ab

300 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

-0.0003

-

-

-

-

-

2901493-001 p-Xylene A1

0.0226

1.49

1.00

1.00

1.49

1.46

2901493-001 p-Xylene A2

0.0219

1.44

1.00

1.00

1.44

2901493-001 p-Xylene B1

0.0219

1.44

1.00

1.00

1.44

1.42

2901493-001 p-Xylene B2

0.0214

1.41

1.00

1.00

1.41

2901493-001 p-Xylene C1

0.0218

1.43

1.00

1.00

1.43

1.44

2901493-001 p-Xylene C2

0.0219

1.44

1.00

1.00

1.44

Mean value :

1.4

Standard deviation (S.D.) :

0.03

Relative Standard Deviation (RSD%):

1.78%

 

(1) Quantification with the lowest standard calibration curve (WSS 1).


 

TABLE 9 Linear calibration for Acetone

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 330 nm

0.0134

0.0594

0.5180

2nd series 330 nm

0.0125

0.0611

0.5153

Mean

0.0129

0.0603

0.5167

Delta

0.0009

0.0017

0.0027

Delta %

7.02%

2.82%

0.53%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0048

0.0086

1.00000

 

TABLE 10 Results obtained for Acetone solubility

 

ChemService

code

As – Ab

330 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

0.0011

-

-

-

-

-

2901493-001 Acetone A1

0.0432

7.16

1.00

1.00

7.16

7.21

2901493-001 Acetone A2

0.0436

7.25

1.00

1.00

7.25

2901493-001 Acetone B1

0.0428

7.09

1.00

1.00

7.09

7.02

2901493-001 Acetone B2

0.0422

6.96

1.00

1.00

6.96

2901493-001 Acetone C1

0.0411

6.73

1.00

1.00

6.73

6.70

2901493-001 Acetone C2

0.0409

6.68

1.00

1.00

6.68

Mean value :

7.0

Standard deviation (S.D.) :

0.23

Relative Standard Deviation (RSD%):

3.36%

 

(1) Quantification with the linear calibration curve.


 

TABLE 11 Linear calibration for Ethyl Acetate

 

Algea Fert Solid K+

WSS 1

1.05mg/mL

(peak area)

WSS 2

10.52mg/mL

(peak area)

WSS 3

105.20mg/mL

(peak area)

1st series 275 nm

0.0175

0.1009

0.8602

2nd series 275 nm

0.0176

0.0907

0.8587

Mean

0.0175

0.0958

0.8595

Delta

0.0001

0.0102

0.0016

Delta %

0.35%

10.67%

0.18%

y = mx + q

Parameterm

(slope)

Parameterq

(intercept)

ParameterR

(correlation)

0.0081

0.0099

1.00000

 

TABLE 12 Results obtained for Ethyl Acetate solubility

 

ChemService

code

As – Ab

275 nm

Cs (1)

(mg/mL)

Ve x Ds

(mL)

Vs

(mL)

Solubility

(mg/mL)

Solubility

Mean

(mg/L)

Control

0.0002

-

-

-

-

-

2901493-001 AcOEt A1

0.0884

9.72

1.00

1.00

9.72

9.63

2901493-001 AcOEt A2

0.0870

9.55

1.00

1.00

9.55

2901493-001 AcOEt B1

0.0853

9.34

1.00

1.00

9.34

9.26

2901493-001 AcOEt B2

0.0841

9.18

1.00

1.00

9.18

2901493-001 AcOEt C1

0.0813

8.84

1.00

1.00

8.84

8.07

2901493-001 AcOEt C2

0.0689

7.30

1.00

1.00

7.30

Mean value :

9.0

Standard deviation (S.D.) :

0.88

Relative Standard Deviation (RSD%):

9.78%

Applicant's summary and conclusion

Conclusions:
From the experimental data obtained according to CIPAC method MT 181 and to guideline A.6 in Official Journal L 383 Part A, it can be concluded that the solubility of the analyzed Algea Fert Solid K+ sample in six organic solvents at room temperature is the following:


Solubility in Methanol : 250.6 mg/L
Solubility in Dichloromethane : 9.9 mg/L
Solubility in n-Hexane : <1 mg/L
Solubility in p-Xylene : 1.4 mg/L
Solubility in Acetone : 7.0 mg/L
Solubility in Ethyl Acetate : 9.0 mg/L