3β-hydroxyandrost-5-en-17-one acetate

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 August 2017 to 23 August 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Version / remarks:

ISO 13320-1

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Specific details on test material used for the study:

- Batch n°: M16GB2547
- Purity: 99.6 % (w/w) (based on assay of T008506)
- Test item storage: At room temperature
- Stable under storage conditions until: 01 July 2018 (retest date)

Mass median aerodynamic diameter:

9.06 µm

Geometric standard deviation:

>= 1.985 - <= 1.992

Percentile:

D10

Mean:

3.462 µm

St. dev.:

0.009

Remarks on result:

other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Key result

Percentile:

D50

Mean:

8.412 µm

St. dev.:

0.034

Remarks on result:

other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Percentile:

D90

Mean:

18.022 µm

St. dev.:

0.163

Remarks on result:

other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Visual Microscope Analysis

(1) Standard visual observation: sample observed to be a fine white powder with clusters.

(2) Observation using 3.2 objective lens: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 22 µm)

(3) Observation using 40 objective lens: sample was observed to be made up of single crystalline particles.

 

Laser Diffraction Particle Size Analysis

Using the identified parameters, the particle size was analysed over the range 0.02μm to 2000μm.

The average Volume weighted Mean was 9.726 µm and the mode was 9.079 µm. The Coefficient of Variation for d50 was <3%; d10 and d90 were <5%. Thus the repeatability of the characteristic particles in the size distribution was within the acceptable limits according to the ISO 13320-1 test standard.

Conclusions:

Visual examination using 3.2 objective lens showed irregular shaped crystals between approximately 3 µm and 22 µm.
The particle size distribution of T008506 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 9.726 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 9.060 µm, whereas the average D10, D50 and the D90 were determined to be 3.462 µm, 8.412 µm and 18.022 µm, respectively.

Description of key information

The particle size distribution of T008506 was determined by the laser diffraction method in a GLP study according to Chilworth Technology Ltd SOP n°417, ISO 13320:2009 and CIPAC MT 187 (Ciric, 2017). The visual examination using 3.2 objective lens showed irregular crystals between approximately 3 µm and 22 µm. The MMAD was determined to be 9.060 µm, whereas the average D10, D50 and the D90 were determined to be 3.462µm, 8.412 µm and 18.022 µm, respectively.