Pharmaceutical Sampling is the involvement of the task designed to select some part of a product for a decided purpose. The Sample is a part of a material collected according to a defined sampling procedure. A Sampling plan describes the location, the number of units and quantity of material that should be collected, and associated acceptance criteria. The Sampling procedure is the complete sampling operations performed on a defined material for a specific purpose. A Sampling unit is a Discrete part of a consignment such as an individual package, drum, or container.
Types of Pharmaceutical Samples
Original Sample is the Sample collected directly from the material.
Combined or Pooled Sample: Sample from all combined parts.
Final Sample: final Sample is the one ready for utilization for the test method.
Random Sample: A sample in which the different portions of the material have an equal possibility of being characterized.
Representative Sample: The sample obtained is consistent with a sampling procedure designed to ensure that the various parts of a batch or the various properties of a non-uniform material are proportionately represented.
Retention sample: The retention sample is collected as a part of the initial sampling process and reserved for further testing in the future. The retention sample size should be sufficient to allow for at least two confirmatory analysis. In some cases, statutory regulations may have more than one Sample, each of which should be separate, determined, packed, and sealed.
Purpose of Pharmaceutical Sampling
Pharmaceutical Sampling is required for different purposes like Prequalification, Acceptance of consignments, Batch release, testing in-process control, Special controls, Inspection for customs clearance, Deterioration, or adulteration.
The test applied for the Retention sample may include:
- Verifying the identity
- Performing complete pharmacopoeial or analogous testing
- They are performing special or specific tests.
Types of Pharmaceutical Products
- Starting materials are used in the manufacture of finished products
- Intermediates are the during the manufacturing process (e.g., bulk granule)
- Pharmaceuticals products (during in-process along with before and after pack)
- Packing materials like primary and secondary materials and cleaning agents
- Compressed gases
- Other processing agents.
Design of Pharmaceutical Sampling Facility
Pharmaceutical Sampling facilities should be designed to prevent contamination of the pharmaceutical intermediates, and in-process containers to prevent cross-contamination from other materials, products, and the environment. Protection to the sampler, which is doing the sampling process.
Preparation for sampling
The sampler should wear gowning for protection during tasks. The sample storage areas must have an adequate light condition, and ventilation care should be taken to guard against the collapse of stacked containers or solids in bulk. The safety data sheet (MSDS) for a pharmaceutical product and related materials).
A sampling of uniform starting materials includes
- Different types of pipettes fitted with suction bulbs, cups or beakers, dippers, and funnels are needed for liquids of low viscosity.
- An inert rod can be used for highly viscous liquid, and spatulas or scoops are a must for powdered and granular solids.
- Sterile products should be sampled under aseptic conditions and only when allowed essentially to prevent the risk of sterility loss.
The use of glass should be avoided.
A sampling of non-uniform materials:
- A sampling tube and a shutter at the lower part may sample liquids in containers or other large-volume containers. A Slotted tube with a pointed part may be used for the solids sample.
Note: All Pharmaceutical sampling tools and implements should be made of inert materials and kept carefully and clean after use or before reuse. They should be thoroughly washed, rinsed with water or a suitable solvent, and dried. All procedures of cleaning should be recorded and documented online.
Sampling Operation and Precautions
Written procedures describing the Pharma sampling operation ensure that representative samples are taken in sufficient quantities for testing according to specifications. The samples should never be returned to the bulk container. The sampling procedure should be followed and monitored, and attention should be paid to any signs of nonconformity of the material. ¨Signs of non-uniformity include
- Variation in particles in shape, size, or color, crystalline, granules, or powdered solid materials;
- Moist crusts on hygroscopic materials;
- Deposits of the solid product in liquid or semi-liquid products; and a layer of liquid products.
Avoid pooling samples from different portions because this will mask contamination, low potency, or other quality problems.
Labeling should be easily identified with relevant details on labels, including the batch number and, if known, the container number from which the Sample was taken, and the amount taken. If a container has been punctured to take a sample, the sampling hole should be appropriately closed and identified as a sampling hole.
Samples containers shall make it should be identified, as they may no longer contain the quantity of product stated on the label. RLAF of the sampling booth should be switched on at least 15 minutes before starting the sampling; only one batch should be sampled at one time.
Containers for Pharmaceutical Samples
The container for storing a sample should not interact with the sampled material nor allow contamination. Bottles closed by screw tops with the inert liners should be for Liquid samples that provide suitable vapor-proof light-sensitive materials and should be protected by using amber glass containers or by using dark-colored foil.
Headspace should be kept to a minimum to reduce any possible degradation. Solid dosage forms like tablets or granules should be protected during transit by filling the container with materials or filling any residual space with a suitable material. Use provided storage conditions to store samples.
Types of Sampling Plans in Pharmaceutical
n Plan: Assuming a uniform material from an identified source with the primary purpose of checking the identity.
Note: “n-plan” is not statistically based and will be used only as a per guideline.
Material to be sampled is taken into account uniformly and is supplied from a recognized source. Samples are often withdrawn from any part of the container (usually from the top layer) by using the formula; n = 1 + √N, where N is the number of sampling units in the consignment. The value of n is obtained by simply rounding n if N is a smaller amount than or up to 4, then every container is sampled. Sampling units are selected randomly, and these are subsequently placed in separate sample containers. The control laboratory inspects the looks of the material and tests the identity of every original Sample consistent with the relevant specification.
p Plan: The material is uniform, is received from a recognized source, and the primary purpose is to test for identity. Formula p = 0.4 under the root of N, where N (number of sampling units). The figures for the p plan are obtained by rounding up to the next highest integer. Samples are withdrawn from each or every N sampling unit of the consignment and kept in divided containers. These samples are to be transferred to the control laboratory, visually inspected, and tested for identity. If the results are satisfactory, p final samples are formed by appropriate pooling of the original samples.
r Plan: The material is suspected to be non-uniform and is received from a poorly known source. Formula r = 1.5 √ N, where N= number of sampling units. The figures for r are determined by rounding up to the next highest integer. Samples are withdrawn from each or every N sampling unit of the consignment and kept in divided containers. These samples are to be transferred to the control laboratory and tested for identity. If the results are satisfactory, r samples are randomly selected and individually subjected to testing. If these results are satisfactory, the r samples are combined for the retention sample.