Reaction product of {mixture of [poly(1~4)chlorosulfonylphthalocyaninato-N29,N30,N31,N32]copper(Ⅱ) and [poly(1~3) chlorosulfonyl (tribenzo[b,g,l]pyrido[2,3-q]-5,10,15,20-tetraazaporphyrinato-N21,N22,N23,N24)] copper(Ⅱ) and [poly(1~2) chlorosulfonyl (dibenzo[b,g(or b,l)]dipyrido [2,3(or 3,2)-l,q(or g,q)]-5,10,15,20-tetraazaporphyrinato-N21,N22,N23,N24)] copper(Ⅱ) and [monochlorosulfonyl (benzo[b]tripyrido [2,3(or 3,2)-g,l,q]-5,10,15,20-tetraazaporphyrinato-N21,N22,N23,N24)]copper(Ⅱ) }and 2-[4-(2-aminoethylamino)-6-(benzylamino)-1,3,5-triazin-2-ylamino]benzene-1,4-disulfonic acid, and ammonia water and sodium chloride

Hydrolysis

Administrative data

Endpoint:

hydrolysis

Type of information:

experimental study

Adequacy of study:

key study

Study period:

11 February 2011 – 27 April 2011

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: This study has been performed according to OECD and EC guidelines and in compliance with GLP principles.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2011

Report date:

2011

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 111 (Hydrolysis as a Function of pH)

Version / remarks:

(2004)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method C.7 (Degradation: Abiotic Degradation: Hydrolysis as a Function of pH)

Version / remarks:

(Official Journal of the European Union no. L142, May 31, 2008)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Test material

Test material information

Constituent 1

Reference substance name:

E-C104

IUPAC Name:

E-C104

Details on test material:

- Name of test material (as cited in study report): E-C104
- Description: Blue powder
- Batch: MB-1
- Test substance storage: At room temperature protected from light
- Stability under storage conditions: Stable
- Expiry date: 23 December 2015

Radiolabelling:

no

Study design

Analytical monitoring:

yes

Details on sampling:

The concentration of the test substance in the test samples was determined immediately after preparation (t=0) and after 5 days. The samples taken at t=5 days were cooled to room temperature using running tap water. The samples were diluted by a factor of 2.5 with buffer pH 4, 7 or 9 and analysed.

Buffers:

- pH: 4
- Type and final molarity of buffer: Acetate buffer, 0.1 M
- Composition of buffer: solution of 16.6% 0.1 M sodium acetate and 83.4% 0.1 M acetic acid. The buffer contains 0.0009% (w/v) sodium azide.

- pH: 7
- Type and final molarity of buffer: Phosphate buffer, 0.1 M
- Composition of buffer: solution of 0.1 M potassium dihydrogenphosphate adjusted to pH 7 using 10 N sodium hydroxide. The buffer contains
0.0009% (w/v) sodium azide.

- pH: 9
- Type and final molarity of buffer: Borate buffer, 0.1 M
- Composition of buffer: solution of 0.1 M boric acid and 0.1 M potassium chloride adjusted to pH 9 using 10 N sodium hydroxide. The buffer
contains 0.0009% (w/v) sodium azide.

Details on test conditions:

Preliminary test - Tier 1:

Test substance solutions were prepared in the buffer solutions at a target concentration of 1000 mg/l. Each solution was filter-sterilised through a 0.2 μm FP 30/0.2 CA-S filter (Whatman, Dassel, Germany) and transferred into a sterile vessel. To exclude oxygen, nitrogen gas was purged through the solution for 5 minutes. For each sampling time, duplicate sterile vessels under vacuum were filled with 6 ml test solution and placed in the dark in a temperature controlled environment at 49.9°C +/- 0.2°C.

Blank buffer solutions were treated similarly as the test samples and analysed at t=0.

The pH of each of the test solutions (except for the blanks) was determined at each sampling time.

Duration of test

Duration:

5 d

Initial conc. measured:

> 952 - < 1 017 mg/L

Number of replicates:

2 measurements at each pH (separate vessels)

Results and discussion

Preliminary study:

At pH 4, pH 7 and pH 9, a degree of hydrolysis of < 10% was observed after 5 days. It demonstrated that the half-life time of the test substance at 25°C is > 1 year. According to the guideline, no further tests were required.

No test substance was detected in blank buffer solutions.

Test performance:

The mean recoveries of the buffer solutions fell within the criterion range of 90-110%. It demonstrated that the analytical method was adequate to support the hydrolysis study on the test substance.

Transformation products:

no

Total recovery of test substance (in %)

Total recovery of test substance (in %) 1

% Recovery:

>= 97 - <= 98

pH:

4

Temp.:

49.9 °C

Duration:

5 d

Total recovery of test substance (in %) 2

% Recovery:

>= 99 - <= 101

pH:

7

Temp.:

49.9 °C

Duration:

5 d

Total recovery of test substance (in %) 3

% Recovery:

>= 98 - <= 99

pH:

9

Temp.:

49.9 °C

Duration:

5 d

Dissipation DT50 of parent compound

Key result

pH:

7

Temp.:

25 °C

DT50:

> 1 yr

Any other information on results incl. tables

Preliminary test – hydrolysis of the test substance at pH 4, pH 7 and pH 9 measured at 268 nm

 

pH code	Sampling time	Analysed concentration [mg/l]	Degree of hydrolysis [%]		Actual pH
			Individual	Mean
pH 4	0 hours	955			4.0
		967			4.0
	5 days	955	0.6	0.1	4.0
		966	-0.5		4.0
pH 7	0 hours	1013			7.1
		1017			7.1
	5 days	1033	-1.8	-1.2	7.1
		1021	-0.6		7.1
pH 9	0 hours	1015			9.0
		1012			9.0
	5 days	1027	-1.3	-1.1	9.0
		1023	-0.9		9.0

 

Preliminary test – hydrolysis of the test substance at pH 4, pH 7 and pH 9 measured at 617 nm

pH code	Sampling time	Analysed concentration [mg/l]	Degree of hydrolysis [%]		Actual pH
			Individual	Mean
pH 4	0 hours	952			4.0
		970			4.0
	5 days	954	0.7	0.7	4.0
		954	0.7		4.0
pH 7	0 hours	1000			7.1
		1011			7.1
	5 days	1014	-0.9	-0.6	7.1
		1010	-0.4		7.1
pH 9	0 hours	1010			9.0
		1007			9.0
	5 days	1004	0.5	0.5	9.0
		1003	0.6		9.0

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

The preliminary test (Tier 1) was performed for the determination of the rate of hydrolysis of E-C104 at pH values normally found in the environment (pH 4-9).

At each pH value a degree of hydrolysis of < 10% was observed after 5 days. According to the guideline, performance of the main study (Tier 2) was not required. The half-life time of the test substance at 25°C was > 1 year at each pH tested.