1,2-Benzenedicarbonitrile, 3-nitro-

Storage stability and reactivity towards container material

Administrative data

Endpoint:

storage stability and reactivity towards container material

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Study Experimental phase 2013-10-28 to 2014-01-06. Study report complete 2014-05-23.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Meets the criteria for classification as Reliable without Restriction according to Klimisch et al (1997).

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2014

Report date:

2014

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

CIPAC MT 46.3 (Storage Stability)

Deviations:

no

GLP compliance:

yes

Type of method:

accelerated testing

Test material

Test material information

Constituent 1

Reference substance name:

-

EC Number:

450-650-8

EC Name:

-

Cas Number:

51762-67-5

Molecular formula:

C8H3N3O2

IUPAC Name:

3-nitrobenzene-1,2-dicarbonitrile

Specific details on test material used for the study:

Reactivials with inert tops were filled with the Test Item, in duplicate, to give minimum headspace. The vials were then sealed with tape and labelled before weighing. A blank vial was also prepared.

After 14 days incubation at 54 +/- 2ºC the vials were removed from storage and left to equilibrate to room temperature before the appearance and weight of the vials were recorded. The tests were then kept in the dark prior to analysis.

The strength and impurity profile of the Test Item after storage was also determined by HPLC. In the absence of any appropriate reference material, the stability test material was compared with the Test Item stored at ambient temperature.

Approximately 40- 50mg of the Test Item was accurately weighed in duplicate, into 100.0 ml volumetric flasks and approximately 80 ml of diluent was added and sonicated to dissolve the sample and cooled to room temperature prior to making to volume and diluting to the mark with diluent (Standards 1 and 2). Then 1.0 ml of this solution was diluted to 10.0 ml with diluent (Standards 1A and 2A). Standard 1A was used to calibrate the instrument and calculate the relative amount of the Test Item present in the test and Standard 2A was used as check standard.

Individual weights taken:
Standard 1: 49.97mg
Standard 2: 40.64m
Test 1 was used for the sample preparation, in duplicate; the same preparation as the standards was performed.
Weights taken:
Test 1 (1 ): 40.99mg
Test 1 (2): 40.03mg

Results and discussion

Results:

The accelerated storage strength of the Test Item after 14 days at 54ºC +/- 2ºC is 99.4% w/w of unstressed Test Item.

The weight loss of the test item was consistent with the weight loss of the blank vial and therefore not considered significant.

No change in the appearance of the test item was noted.

The% RSD of the area of 5 injections of Standard 1A was within the 5% acceptance criteria and the % RSD of the retention times was also within the 1% acceptance criteria. Therefore the suitability of the method was confirmed.

The impurity profile of the Test Item after 14 days at 54°C ± 2°C is the same as the unstressed sample.

Applicant's summary and conclusion

Conclusions:

The accelerated storage strength of the Test Item after 14 days at 54ºC +/- 2ºC is 99.4% w/w of unstressed Test Item. Over the test time period the test material has been shown to be stable. Therefore, there has not been any significant active ingredient degradation and according to CIPAC MT 46 this indicates an ambient shelf life of at least 2 years.

Executive summary:

Introduction

This study was undertaken to assess the storage stability of the test material.

Results & Conclusions

The weight loss of the test item was consistent with the weight loss of the blank vial and therefore not considered significant. No change in the appearance of the test item was noted. The accelerated storage strength of the Test Item after 14 days at 54ºC +/- 2ºC is 99.4% w/w of unstressed Test Item. Over the test time period the test material has been shown to be stable. Therefore, there has not been any significant active ingredient degradation and according to CIPAC MT 46 this indicates an ambient shelf life of at least 2 years.