Stability Operating Procedures sample

Every company must have a written stability program documented in a standard operating procedure (SOP). This program will define the requirements for stability studies to be put up to assess the stability profile and the expiry of the drug product. It is required to have the sample sizes and testing intervals defined along with storage... 

This chapter introduces day-to-day activities necessary to a successful stability program. It explains critical activities as well as most common practices to manage stability studies from the time that samples are delivered to the stability laboratories to the time that study ends. These activities are usually written into Standard Operating Procedures (SOPs). Many companies have a dedicated group of analysts to manage these operations. 

The data required for a kinetic formulation of the deactivation of the main reaction are probably best collected in a differential reactor. Some extrapolation to zero time is required when the reaction rate of the main reaction cannot be observed at zero coke content. The procedure can be hazardous with very fast coking, of course. In their study of butene dehydrogenation, Dumez and Froment [1976] were able to take samples of the exit stream of stabilized operation of the fixed bed reactor after 2 minutes, while the observations extended over more than 30 minutes. 

When glycerol is nitrated for use in military smokeless propellants, the main requirement is usually not the yield of NG, but its stability and other properties, as required by the specifications. If this is the case, a smaller sample can be used (10g), but the nitrating acid should be prepd from technical acids used in the plant and not from cp acids Following is a procedure originated by Hercules Powder Co and adopted at Pica tinny Arsenal with slight modifications. All operations should be conducted behind safety ass Reagents ... 

What constitutes a significant difference between two spectra When the differences are small, the answer depends on sample preparation and sample stability as well as accuracy of concentration determination, identification of and compensation for drift in the spectrometer, correct baseline correction, absence of bubbles in the sample, reproducible cleanliness of the cuvette, and the level of general handling procedures. Ultimately, an assessment of significance depends on the experience, competence, and confidence of the operator. 

We successfully applied an AChE inhibition assay to the detection of dichlorvos in durum wheat samples using a simplified extraction procedure. The total assay time, including the extraction step, was 30 min. Considering that several extractions and assay steps can be run simultaneously, the throughput for one operator is 12 determinations per hour. It is also important to stress that the choline oxidase biosensor used in this work showed an excellent functioning stability after 20 days from preparation, the blank measurement lost only 10% of the signal intensity. The method allowed the accurate analysis of dichlorvos in wheat samples at the MRL, 2 mg/kg, and below that value. The mean recovery was 75%, and neither false nor positive samples were detected. Finally, the portable electrochemical instrumentation combined with the simple extraction procedure was quite well suited for in situ analysis of dichlorvos in durum wheat. 

At the same time, internal quality control must be carried out to verify the performance stability of the limited-scope performance of the method. Triply redundant verification methods are carried out with regard to control of first, second and/or third line, each set of methods applied to a particular type of test. The first line of verification involves pro forma repetition of all the steps of the test, in order to establish repeatability or reproducibility for quantitative tests, and to verify the range of sensitivity or detection for qualitative tests. This verification is performed by the experimenter himself, as part of the proper performance of the test. A second line of verification is put into operation by administrative decision, and includes testing with blind samples, repetition of samples, internal audit procedures, etc. If necessary, a third line of verification can be set up by the use of certified reference materials (or spiking materials), or through collaborative trials. These procedures are based on external cooperation. External audit procedures and complaints handling procedures are also part of this third line of verification. 

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