To lay down the procedure for sampling of intermediates, drug substances, drug products.
2. Scope :
This procedure is applicable for Pharmaceutical Industry of API as well as formulations.
3. Definition :
- Sample: Sample is a portion of a material collected according to a deﬁned sampling procedure. The size of any sample should be sufficient to allow all anticipated test procedures to be carried out, including all repetitions and retention samples.
4. Responsibility :
Quality Control, Quality Assurance
5. Procedure :
5.1 Sampling Process:
- Sampling may be required for different purposes, such as pre-qualiﬁcation; acceptance of consignments; batch release testing; in-process control; special controls; inspection for customs clearance, deterioration or adulteration; or for obtaining a retention sample.
- The tests to be applied to the sample may include:
-Verifying the identity;
-Performing complete pharmacopoeial or analogous testing; and
-Performing special or speciﬁc tests.
5.2 Preparation for Sampling for the Sampling of Products
- The responsible person should have at his or her disposal all the tools needed to open the containers (e.g. packages, barrels and others).
- Tools may include knives, pliers, saws, hammers, wrenches, implements to remove dust (preferably a vacuum cleaner), and material to reclose the packages (such as sealing tape), as well as self-adhesive labels to indicate that some of the contents have been removed from a package or container.
- Containers to be sampled should be cleaned prior to sampling if necessary. Sampling of uniform starting materials does not require complicated tools.
- A variety of pipettes ﬁtted with suction bulbs, cups or beakers, dippers and funnels are needed for liquids of low viscosity. The use of glass should be avoided.
- A suitable inert rod can be used for highly viscous liquid, and spatulas or scoops are needed for powdered and granular solids.
- Sterile pharmaceutical products should be sampled under aseptic conditions, and only when deemed absolutely essential, to avoid the risk of loss of sterility.
- The tools for sampling non-uniform materials are more complicated and more difficult to clean.
- It is important to follow the manufacturer’s instructions for the use of sampling devices.
- All sampling tools and implements should be made of inert materials and kept scrupulously clean.
- After use or before reuse, they should be thoroughly washed, rinsed with water or suitable solvent, and dried.
- They should be stored in clean conditions.
- Adequate washing facilities should be provided in, or in close proximity to, the sampling area, otherwise samplers will need to bring separate clean sets of implements for sampling each product.
- The cleaning procedure used for all sampling tools and implements should be documented and recorded.
- The adequacy of the cleaning procedure for the material from which the sampling tool is made should be demonstrated. The use of disposable sampling materials has distinct advantages.
5.3 Sampling Operation and Precautions
- There should be a written procedure describing the sampling operation.
- This should include details of the health and safety aspects of sampling also.
- It should ensure that representative samples are taken in sufficient quantity for testing in accordance with speciﬁcations.
- Closures and labels should preferably be such that unauthorized opening can be detected. Samples should never be returned to the bulk.
- The sampling process should be appropriately supervised and documented
- The sampling procedure should be such that non-uniformity of the material can be detected.
- During the sampling procedure, attention should be paid to any signs of nonconformity of the material.
- Signs of non-uniformity include differences in shape, size or colour of particles in crystalline, granular or powdered solid substances; moist crusts on hygroscopic substances; deposits of solid pharmaceutical product in liquid or semi-liquid products; and stratiﬁcation of liquid products.
- Such changes, some of which may be readily reversible, can occur during prolonged storage or exposure to extreme temperatures during transportation.
- Homogeneous portions of the material or bulk such as those mentioned above should be sampled and tested separately from the rest of the material that has a normal appearance.
- Pooling of the samples from the different portions should be avoided, because this can mask contamination, low potency or other quality problems.
- Labeling of samples should provide appropriate details, including the batch number and, if known, the container number from which the sample was taken, the amount taken and for what purpose.
- Labels should be applied at the time of sampling. The container used to store the sample should also be properly labeled with appropriate details such as sample type, name of material, identiﬁcation code, batch/lot number, code, quantity, date of sampling, storage conditions, handling precautions and container number.
- For ﬁnished drug products, the sampling procedure should take account of the ofﬁcial and non-ofﬁcial tests required for the individual dosage form (e.g. tablets or parenteral preparations).
- Non-ofﬁcial tests could include testing for adulteration and counterfeiting. The sampling procedure should also take account of past experience with the pharmaceutical product or related material and with the supplier, and of the number of sampling units in the consignment.
- When a container is sampled outside the control of the consignee of the product, the following precautions should be taken.
- If the tamperproof seal is broken to obtain a sample, then the consignee of the product should be informed and the container resealed with an appropriate tamper-proof seal, and the consignee of the product informed of its type and its identiﬁcation.
- If a bag has been punctured to take a sample, then the sampling hole should be appropriately closed and identiﬁed as a sampling hole made by an authorized sampler.
- Sampled containers should be identiﬁed, as they may no longer contain the quantity of product stated on the label.
5.4 Storage and Retention
- The container used to store a sample should not interact with the sampled material nor allow contamination.
- It should also protect the sample from light, air and moisture, as required by the storage directions for the pharmaceutical product or related material sampled.
- As a general rule, the container should be sealed and preferably tamper-evident.
- Samples of loose materials, whether solid or liquid, should be placed in one or more clean containers.
- Liquid samples should be transported in suitable bottles closed by screw tops with inert liners that provide a good vapour-proof (moisture-proof) seal for the contents.
- Suitable screw-top jars in exceptional cases only should be used for solid or semi-solid pharmaceutical products. The container should be inert.
- Light-sensitive materials should be protected by using amber glass containers or by wrapping colorless glass containers in foil or dark-colored paper.
- Headspace should be kept to a minimum to minimize any possible degradation. for example, nitrogen gassing.
- Solid dosage forms such as tablets or granules should be protected during transit, either by totally ﬁlling the container with the product or by ﬁlling any residual space with a suitable material.
- All containers should be sealed and labelled, and all samples should be packaged adequately and transported in such a way as to avoid breakage and contamination during transport. For all containers that come apart (e.g. screw-capped jars or metal tins with separate lids) precautions should be taken to avoid any mix-up when they are opened for examination, such as by labeling all parts of each container whenever possible.
- If one sample is divided into several sample containers, they should be transported in a suitably sealed box, which should be labeled with the identity of the product, the consignment from which the sample was drawn, the size of the sample, the date and place of sampling, and the name of the inspector.
- Security and adequate storage conditions should be ensured for the rooms in which samples are stored. Samples should be stored in accordance with the storage conditions as speciﬁed for the respective active pharmaceutical ingredient (API), excipient or drug product. Packaging materials similar to those in which the bulk is supplied should be used for long-term storage.
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