Benzenesulfonic acid, 4-[(1,3-dioxobutyl)amino]-, sodium salt (1:1)

Short-term toxicity to aquatic invertebrates

Administrative data

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: well performed OECD study with GLP

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2015

Report date:

2015

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

no

GLP compliance:

yes

Test material

Test material information

Constituent 1

Reference substance name:

sodium 4-(3-oxobutanamido)benzene-1-sulfonate

EC Number:

613-240-1

Cas Number:

63503-98-0

Molecular formula:

C10H11NO5S.Na

IUPAC Name:

sodium 4-(3-oxobutanamido)benzene-1-sulfonate

Test material form:

other: Grey lumps

Sampling and analysis

Analytical monitoring:

yes

Details on sampling:

The limit concentration and the control were analytically verified via HPLC-DAD at the start of the exposure (0 hours) and at the end of the exposure (48 hours) as specified below.
At the start of the exposure (0 hours), samples were taken immediately after preparation of the limit concentration and analysed.
At the end of the exposure (48 hours), samples were taken directly from the test vessels of the limit concentration and the control and analysed.
The method was validated according to SANCO 3029/99 rev.4 (2000).


Recoveries of the test item should be within ± 20 % of the nominal or initially measured concentration.
The effect levels can be given based on the nominal concentrations, if this quality criteria is fulfilled.

Test solutions

Vehicle:

no

Details on test solutions:

Preparation of the The stock solution (100 mg/L of the test item were weighed out)
saturated solution was freshly prepared with ISO test water before the start of the exposure interval (0 hours).

Treatment Agitation

Test organisms

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Daphnia magna
- Strain: Clone 5
- Source:
Origin: Institut für Wasser-, Boden- und Lufthygiene (WaBoLu)
Breeder: DR.U.NOACK-LABORATORIEN, Käthe-Paulus-Str. 1, 31157 Sarstedt, Germany
- Age at study initiation (mean and range, SD): 2 to 24 h old daphnids from a healthy stock were used for the study
- Method of breeding:
Culture: In glass vessels (2 - 3 L capacity) with approximately 1.8 L culture medium, at 20 +- 2°C, in an incubator, 16 h illumination; light intensity
of max. 20 µE x m-2 x s-1
Culture medium: Elendt M4, according to ELENDT (1990), modified to a total hardness of 160 to 180 mg CaCO3/L
Cultur feeding: At least 5 times per week ad libitum with a mix of unicellular green algae, e.g. Pseudokirchneriella subcapitata and
Desmodesmus subspicatus, with an algae cell density of > 106 cells/mL
- Feeding during test: No feeding

ACCLIMATION
- Acclimation period: At least 2 h in dilution water.
- Acclimation conditions (same as test or not): Same as test conditions.
- Health during acclimation (any mortality observed): No mortality observed.

Study design

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

48 h

Test conditions

Hardness:

272 mgCaCO3/L

Test temperature:

18 - 22°C, constant within ± 1°C
At start of exposure: 20.9

pH:

pH at the Start of the Exposure (0 hours)
(measured in one additional replicate of the limit concentration and the control)

Nominal test item
concentration
[mg/L] pH-value

100 7.88
Control 7.63


pH at the End of the Exposure (48 hours)
(measured in all replicates)

Nominal test item
concentration
[mg/L] pH-values
Replicates
1 2 3 4
100 7.83 7.84 7.85 7.85
Control 7.64 7.75 7.80 7.82

Dissolved oxygen:

O2-concentration at the Start of the Exposure (0 hours)
(measured in one additional replicate of the limit concentration and the control)

Nomonal test item
concentrations
[mg/L]
Dissolved
O2-concentration
[mg/L]
100 8.55
Control 8.50



O2-concentration at the End of the Exposure (48 hours)
(measured in all replicates)

Nominaltest item
concentrations
[mg/L] Dissolved O2 -concentration [mg/L]
Replicates
1 2 3 4
100 8.50 8.38 8.42 8.40
Control 8.26 8.27 8.30 8.29

Nominal and measured concentrations:

Nominal: 100 mg/L
The measured concentration of the test item was 102 mg/L at the start of the exposure (0 hours) an 97.6 mg/L at the end of the exposure (48 hours).

Details on test conditions:

TEST SYSTEM
- Test vessel: Glass beakers (4 cm ID x 7 cm H), 50 mL capacity, loosely covered with watch glasses
- Test volume: 20 mL
- Aeration: None
- No. of organisms per vessel: 5
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: ISO Test water, according to OECD 202, Annex 3
Component Concentration [mg/L]
KCl 5.76
NaHCO3 64.8
CaCl2 x 2 H2O 294
MgSO4 x 7 H2O 123

- Water Quality Parameters of the Dilution Water prior to the Start of the Exposure (0 h):
pH-value DissolvedO2-concentration[mg/L] Temperature[°C] Conductivity[µS/cm] Total hardness [mg CaCO3/L]
7.63 8.50 20.9 681 272

- Culture medium different from test medium: Elendt M4, according to ELENDT (1990), modified to a total hardness of 160 to 180 mg CaCO3/L
- Intervals of water quality measurement: test start (0h) and test end (48h)

OTHER TEST CONDITIONS
- Photoperiod: 16/8 h light/dark cycle
- Light intensity: Diffuse light, light intensity of max. 20 µE x m-2 x s-1

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :
- Immobilisation, 24 h interval

TEST CONCENTRATIONS
-A limit concentration of the test item of 100 mg/L was tested.

- Range finding study:
A non GLP preliminary range finding test under static conditions over a period of 48 hours was conducted at the test facility with three nominal test item concentrations of 1.00, 10.0 and 100 mg/L. In the range finding test, two replicates per treatment group and control, each with ten daphnids,
were tested. No significant effects were observed at any of the tested concentration levels. The biologically results are presented in the table below.


Immobilisation Rates in the non GLP Preliminary Range Finding Test
(n = 20, divided into 2 replicates with 10 daphnids each)

Nominal
test item
concentration
[mg/L] IMMOBILISATION [%]
24 hours 48 hours
Replicates Replicates
1 2 MV 1 2 MV
100 0 0 0 0 0 0
10.0 0 0 0 0 0 0
1.00 0 0 0 0 0 0
Control 0 0 0 0 0 0


MV = mean value

The exposure concentrations were monitored at the start (0 hours) and at the end (48 hours) of the exposure intervals in test vessel with daphnids
and test vessels without daphnids.
The results of the analytical monitoring during the range finding test are presented in the table below.


Measured Concentrations of Acetessigsulphanilsäure-Natriumsalz, trocken during the non GLP Preliminary Range Finding Test


Sampling date 2015-01-27 2015-01-29

0 hours 48 hours
Start of the exposure End of Exposure

Nominal
test item concentration
Acetessigsulphanilsäure-Natriumsalz, trocken

Meas. conc. Meas. conc.
[mg/L] % [mg/L %

100 102 102 113 113
10.0 9.54 95 9.47 95
1.00 0.956 96 0.955 96
Control < SysQL < SysQL
Meas. conc. = measured concentration of the test item, mean value of 2 injections, dilution factors taken into account
% = percent of the nominal concentration of the test item
SysQL = system quantification limit (0.1 mg/L of the test item)

Reference substance (positive control):

yes

Remarks:

Potassium dichromate

Results and discussion

Effect concentrations

Effect concentrations 1

Duration:

24 h

Dose descriptor:

other: EC10,50,100

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: immobilisation

Effect concentrations 2

Duration:

48 h

Dose descriptor:

other: EC10,50,100

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: immobilisation

Effect concentrations 3

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: immobilisation

Effect concentrations 4

Duration:

48 h

Dose descriptor:

LOEC

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: immobilisation

Details on results:

See below

Results with reference substance (positive control):

The percentage immobility for the reference item was determined after 24 hours. The EC50-value with 95 % confidence limits (CI) was calculated by sigmoidal dose-response regression. The EC50-value for the most recent of the monthly performed reference tests was:
EC50: 1.96 mg/L (CI 1.78 - 2.13 mg/L)
The EC50-value of the reference item potassium dichromate after 24 h is within the prescribed concentration range of 0.6 - 2.4 mg/L of quality criteria according to AQS P 9/2 (02/2000) for daphnids clone 5 cultured in Elendt M4 medium. The EC50-value of the reference item is also within the recommended range of 0.6 - 2.1 mg/L according to OECD-Guideline 202.

Any other information on results incl. tables

Biological Data

The percentage immobility, determined in the limit concentration and the control after 24 and 48 hours under static conditions, is given in the table

below.

Immobilisation Rates after 24 and 48 hours of Exposure in the Definitive Test

 (n = 20, divided into 4 replicates with 5 daphnids each)

Acetessigsulphanilsäure-Natriumsalz, trocken	IMMOBILISATION [%]
Nominal test item concentration   [mg/L]	24 hours					48 hours
	Replicates					Replicates
	1	2	3	4	MV	1	2	3	4	MV
100	0	0	0	0	0	0	0	0	0	0
Control	0	0	0	0	0	0	0	0	0	0

 

The limit concentration was visually clear throughout exposure.

 

Measured Exposure Concentrations during the Definitive Test

The limit concentration of the test item Acetessigsulphanilsäure-Natriumsalz, trocken and the control were analytically verified by HPLC-DAD at the start of the exposure (0 hours) and at the end of the exposure (48 hours).
The measured concentration of the test item was 102 mg/L at the start of the exposure (0 hours) and 97.6 mg/L at the end of the exposure

(48 hours).
The analytical results are presented in the table below.

The recoveries of the test item were within ± 20 % of the nominal value. This indicates that the test item was successfully maintained for the duration of the test.

Measured Concentrations and Percent of the Nominal Concentration of the Test Item Acetessigsulphanilsäure-Natriumsalz,trockenin the Definitive Test

Sampling date	2015-04-21 Start of the exposure, 0 hours		2015-04-23 End of the exposure, 48 hours
Date of analysis	2015-04-23		2015-04-23
Nominal test item concentration [mg/L]	Acetessigsulphanilsäure-Natriumsalz, trocken
	Meas. conc. [mg/L]	%	Meas. conc. [mg/L]	%
100	102	102	97.6	98
Control	< LOQ		< LOQ

Meas. conc.= measured concentration of the test item, mean value of 2 injections, dilution factor taken into account

%                  = percent, related to the nominal test item concentration of the test item

LOQ             = limit of quantification of theanalytical method(1 mg/L of the test item)

 

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

At the limit concentration of 100 mg/L of the test item Acetessigsulphanilsäure-Natriumsalz, trocken, no effects were observed on Daphnia magna.

Executive summary:

In the acute immobilisation test with Daphnia magna (STRAUS), the effects of the limit concentration of 100 mg/L of the test item Acetessigsulphanilsäure-Natriumsalz, trocken was determined according to OECD 202 (2004). The limit test was conducted under static conditions over a period of 48 hours from 2015-04-21 to 2015-04-23, at Dr.U.Noack-Laboratorien, Käthe-Paulus-Str.1, D-31157 Sarstedt, Germany.

The limit concentration of 100 mg/L was visually clear throughout the exposure.

Twenty daphnids were exposed to the limit concentration and the control.

The limit concentration of the test item Acetessigsulphanilsäure-Natriumsalz, trocken and the control were analytically verified by HPLC-DAD at the start of the exposure (0 hours) and at the end of the exposure (48 hours).
The measured concentration of the test item was 102 mg/L at the start of the exposure (0 hours) and 97.6 mg/L at the end of the exposure

(48 hours).

The recoveries of the test item were within ± 20 % of the nominal value. This indicates that the test item was successfully maintained for the duration of the test. Therefore, the effect levels can be based on the nominal concentrations of the test item Acetessigsulphanilsäure-Natriumsalz, trocken.

The water quality parameters (i.e. pH-value and dissolved oxygen concentration), measured at the start (0 hours) and at the end of the exposure

(48 hours), were within the acceptable limits. The validity criteria of the test guideline were fulfilled.

    

EC-Values, NOEC and LOEC (based on the nominal concentration of the test item)

Effect levels	Test duration [h]	Acetessigsulphanilsäure-Natriumsalz, trocken
		Nominal test item concentration [mg/L]
EC10 /50 / 100	24	> 100
	48	> 100
NOEC	48	100
LOEC	48	> 100