content_image/943429.jpg content_image/943433.jpg content_image/943432.jpg content_image/943431.jpg content_image/943430.jpg
gently swirled or inverted, ensuring that air bubbles are not introduced, and observed for about 5 s in front of the white panel. The procedure is repeated in front of the black panel. The presence of any particles is recorded. 

[0172] The visual scores are ranked as follows: 

[0173] Visual score 1: Clear solution, virtually free of particles 

[0174] Visual score 2: - 5 very small particles 

[0175] Visual score 3: - 10-20 very small particles 

[0176] Visual score 4: 20-50 particles, including larger particles 

[0177] Visual score 5: >50 particles, including larger particles 

[0178] Whilst the particles in samples with visual scores 4 and 5 are clearly detectable on casual visual assessment under normal light, samples with visual score 1-3 generally appear as clear solutions on the same assessment. Samples with visual scores 1-3 are considered to be "Pass"; samples with visual score 4-5 are considered to be "Fail" 

( c) Size Exclusion Chromatography 

[0179] Ultra-high performance size exclusion chromatog› raphy of insulin preparations was performed using the Waters ACQUITY H-class Bio UPLCfi system with a 1.7 µm Ethylene Bridged Hybrid 125 A pore packing material in a 300 mm by 4.6 mm colunm. The column was equilibrated in 0.65 mg/ml L-arginine, 20% v/v acetonitrile, 15% v/v glacial acetic acid mobile phase and 10 µI of sample, acidified with 0.01M HCI, was analysed at 0.4 mL/min, with 276 nm UV detection. All analyses were performed at ambient temperature. Results are expressed as % high molecular weight species (HMWS) with respect to the total protein content. 

( d) Reversed-Phase Chromatography 

[0180] Ultra-high performance reverse phase chromatog› raphy was performed using the Waters ACQUITY H-class Bio UPLCfi system with a 1.7 µm Ethyene Bridged Hybrid particle, 130 A pore resin trifunctionally immobilised with a C18 ligand in a 50 mm by 2.1 mm colunm. Insulin samples were bound in a 82% w/v Na$_{2}$ SO$_{4}$ , 18% v/v acetonitrile, pH 2.3 mobile phase and eluted in 50% w/v Na$_{2}$ SO$_{4}$ , 50% v/v acetonitrile gradient flow. 2µ1 of sample was acidified with 0.01M HCI and analysed at 0.61 mL/min, with 214 nm UV detection. All analyses were performed at 40° C. 

[0181] The following example formulations may be pre› pared: 

[0182] 

<img src='content_image/943429.jpg'>

## Example 1 

## Example Formulations 

<img src='content_image/943433.jpg'>

[0183] 

<img src='content_image/943432.jpg'>

[0184] 

<img src='content_image/943431.jpg'>

[0185] 

<img src='content_image/943430.jpg'>

-continued 

