This standard specifies the specifications, technical indicators and requirements, test methods, inspection rules, criterion rule and requirements of product packaging, labeling, transportation and storage of empty pullulan capsules. This standard is applicable to empty pullulan hard capsules made of pullulan and auxiliary materials and pullulan should meet Standard of Pullulan for capsules.
The empty pullulan capsule is a cylindrical hard capsule with a cap and body section, and various locking structures. Capsules are divided into 00#, 0 #, 1 #, 2 #, 3 #, 4 #, 5 # and other special sizes according to their capacity. Conventional extended capsules are represented by el, such as 0# el. Also, the capsule can be divided into three types: transparent (both sections do not contain opacifier), opaque (both sections contain opacifier), and translucent (only one section contains opacifier).
Physical and chemical indicators of capsules
|Identification||-||Conforms to composition|
|Disintegration time||min||≤ 20|
|Loss on drying||%||9.0-14.0|
|Ignition residue (transparent)||%||≤ 2.0|
|Ignition residue (translucent)||%||≤ 3.0|
|Ignition residue (opaque)||%||≤ 5.0|
If ethylene oxide sterilization or the paraben antibacterial agents are used during production, shall add the detection and control of the corresponding project.
|Total Bacterial count||cfu/g||≤ 1000|
|Yeast and Moldscount||cfu/g||≤ 100|
pullulanase solution (10 units/ml), polyethylene glycol 600.
take 10g of the product, add 100ml of water for dissolution, and add the sample while stirring for dissolution process to get a viscous solution. Take 1 tube, add 10ml of viscous solution, add 0.1ml of pullulanase solution (10 units/ml), and then leave the tube for 20 minutes at room temperature. The viscosity of the solution is significantly lower than that of the test solution without enzyme. Take 10ml of viscous solution, dilute to 50ml with water, shake well, take 10ml of it and add 2ml of polyethylene glycol 600, then white precipitate is produced immediately.
Instruments and excipients
a disintegration time tester (temperature is controlled at 37 ± 1 ° C)
take 6 capsules, fill them with talcum powder (the filled capsule shall not float on the water), lock the capsules, and then place capsules in the glass tube of the hanging basket, put on the baffle. All the capsules should be completed disintegrated in 20 minutes, and there should be no other things left on the sieve excepting for the broken capsule shell. If some of the disintegrated capsules cannot pass through the sieve, but they are softened or lightly float on the water, it is also in accordance with the regulations. If one of the capsules does not disintegrate, should test another 6 capsules, and all of them should meet the requirements.
a wooden board (thickness of 2 cm)
take 10 capsules, use the thumb and forefinger to gently pinch the ends of the capsule, rotate and separate the capsules. There should be no sticking, deformation or cracking, then fill capsules with the talcum powder, and lock the capsules. Drop the capsules from the height of 1 m to the wooden board one by one, and there should be no powder leaked. If there is a small amount of powder leakage, the powder should come from one capsule. If exceeding, take another 10 capsules to test, and they should meet the requirements.
Reagents and instruments
saturated magnesium nitrate solution, a desiccator, a glass tube (24 mm of inner diameter, 200 mm of length), PTFE cylindrical weights (diameter of 22 mm, weight of 20.0 ± 0.1 g), and a wood board (thickness of 2 cm).
take 50 capsules, put them in a watch glass, and then move it into a desiccator containing a saturated solution of magnesium nitrate. Place the desiccator under 25 ° C ± 1 ° C for 24 h, then taken out the capsules and immediately put them into a glass tube standing upright on a wooden board separately. The cylindrical weight will freely fall from the opening of the glass tube, and the number of broken capsules shall not exceed 5.
Loss on drying
an analytical balance (accuracy 0.1 mg), a desiccator, a drying oven (the temperature is controlled at 105 ± 2 ° C), and a weighing bottle.
weigh capsules of 1.0 g, separate capsules into caps and bodies, dry them under 105 ° C for 6 h, and the weight lost should not exceed 9.0%~14.0%.
Calculation: y= (m1-m2) / (m1-m0) ×100%
In the formula:
y — loss on drying, %
m1 — the total weight of the weighing bottle and the sample before drying, in grams (g)
m2 — the total weight of the weighing bottle and the sample after drying, in grams (g)
m0 — the weight of the weighing bottle, in grams (g)
The result of the calculation is expressed as one decimal place.
the absolute difference between the two tests under repetitive conditions should be no more than 0.4%.
The measuring method of the residue on ignition, Pb, microorganisms, inspection rules, criterion rule, and product packaging, labeling, transportation, storage requirements are the same as those for empty gelatin capsule standard.