Triglycerides, C16-18 (even numbered), reaction products with diethylenetriamine

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

14 September 2015 - 13 February 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

GLP compliance:

yes (incl. QA statement)

Remarks:

certificate attached to study report

Other quality assurance:

ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)

Type of method:

flask method

Specific details on test material used for the study:

Test item without emulsifier was investigated.

Amidoamine (UVCB)
Pulcra ID: DE07_2014_012_BEL66 (amidoamine without emulsifier)
Physical state: pale yellowish solid at 20 °C
Batch No.: K8 4309 L481
Expiry date of batch: 09 March 2018
Purity: 100 % (UVCB)
Stability: stable under test conditions
Storage condition of test material: Room temperature, protected from light

Key result

Water solubility:

< 0.01 mg/L

Temp.:

20 °C

pH:

> 11

Details on results:

The concentration of test item in the sample solutions was determined by liquid chromatography – mass spectroscopy (LC-MS).

A preliminary test was performed in order to select the appropriate method and to determine the approximate amount of test item to be used in the main test.

An aliquot of ground test item (0.10 g) was added to 500 mL of purified water. After shaking at 30 °C for 24 hours and standing at 20 °C for at least 24 hrs, the mixture was filtered through a 0.45 µm filter to provide a clear supernatant free from excess undissolved test item. An aliquot of the supernatant (100 mL), adjusted to pH > 11 using sodium hydroxide, was passed through a Strata X (100 mg, 6 mL) solid phase extraction (SPE) cartridge, and the test item eluted using 1 mL of methanol/tetrahydrofuran/formic acid (80/20/0.1 v/v/v). The eluate was analysed using the conditions detailed below.

After preparation, the samples were shaken at approximately 30 °C for 24¾, 48 and 72 hours After standing at 20 °C for a period of at least 24 hours, the contents of the flasks were filtered through a 0.45 µm filter to provide a clear supernatant free from excess undissolved test item. The pH of each sample solution was measured.

The concentration of test item in the sample solutions was determined by liquid chromatography – mass spectroscopy (LC-MS).

In duplicate, an aliquot of the supernatant (100 mL), was passed through the SPE cartridge and dried under vacuum for approximately 10 minutes and further dried using nitrogen for approximately 25 minutes. The analyte was eluted using methanol/tetrahydrofuran/formic acid (80/20/0.1 v/v/v, [mobile phase B]) into a 1 mL volumetric flask and vialled for analysis.

Calibration standard solutions of test item were prepared in methanol/tetrahydrofuran/formic acid (80/20/0.1 v/v/v, [mobile phase B]) in the nominal concentration range of 0.1 to 1.5 mg/L.

Matrix Blank was Methanol/tetrahydrofuran/formic acid (80/20/0.1 v/v/v).

The standard, blank and sample solutions were analyzed by LC-MS using the following conditions:

HPLC System : Agilent Technologies 1100 Series

Detector type : Mass selective (MS)

Column : Zorbax Eclipse SB-C3 5µm (250 x 4.6 mm id)

Column temperature : 30 °C

Mobile phase : Mobile phase A: Methanol:water:formic acid 50/50/0.1 v/v/v

Mobile phase B : Methanol:THF:formic acid 80/20/0.1 v/v/v

Flow-rate : 1.0 mL/min

Injection volume : 25 µL

Time (mins)	% A	% B
0	99.9	0.1
7	0.1	99.9
11	0.1	99.9
11.5	99.9	0.1
15	99.9	0.1

MS detector parameters:

Mode: SIM

Mass (m/z)*: 580 (diamide of diethylenetriamine and palmitic acid), 608 (diamide of diethylenetriamine and palmitic and stearic acid), 636 (diamide of diethylenetriamine and stearic acid) - chosen as key components representing > 50 % of the amidoamine test item.

Fragment voltage: 325 V

Polarity: positive

Nebuliser Pressure: 25 psi

Capillary Voltage: 5000

Drying Gas Flow: 6 L/min

Drying Gas Temperature: 275 °C

Retention time : Approximately 9.3 to 9.6 minutes (3 peaks)

The mean peak area and concentration of each standard were plotted on a calibration curve. The concentration of the sample solutions (mg/L) was interpolated from this curve and was corrected for dilution factor (0.01) and a recovery correction factor (1.74).

Sample number	Time shaken at 30 °C (hours)	Time equilibrated at 20°C (hours)	Mean concentration corrected for recovery (g/L)	Solution pH
1	24.75	24.75	6.93 x 10^-4	5.9
2	48	24.75	8.62 x 10^-4	5.9
3	72	24.75	7.03 x 10^-4	6.1

The limit of detection for the analysis was defined as the concentration of the lowest acceptable calibration standard, corrected for recovery, 1.83 x 10-3 mg/L (1.83 x 10-6 g/L).

Conclusions:

Interpretation of results (migrated information): insoluble (< 0.1 mg/L)
The water solubility was determined to be less than 1.02 x 10-5 g/L at 20.0 ± 0.5 °C.

Executive summary:

In the GLP Klimisch 1 key study, the water solubility of amidoamine test item was determined according to OECD 105 and EU method A.6. The water solubility was determined to be less than 1.02 x 10-5 g/L at 20.0 ± 0.5 °C.

Description of key information

Interpretation of results (migrated information): insoluble (< 0.1 mg/L)

The water solubility was determined to be less than 1.02 x 10-5 g/L at 20.0 ± 0.5 °C.

Key value for chemical safety assessment

Water solubility:

0 g/L

at the temperature of:

20 °C