Protocol preparation

If testing involves a new product that is not yet in commercial trade, the manufacturer should ship products from the same batch of the same formulation to each test location. The most recent product quality analysis and an appropriate Material Safety Data Sheet (MSDS) must accompany the product shipment. The shipping documents and the certificate of analysis for each shipment must be archived in the raw data for the report. If the residue testing is being done to register a new use for a commercial product, the Study Director must make sure that the product available in each location is the same formulation and that each different batch encountered has its own certificate of analysis to be archived along with a copy of the label and product quality analysis of the material used for the test. Material shipped in noncommercial containers must 

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The validation process is subject to the following design specifications, user and performance requirements, preparation of a master plan/validation protocol (installation qualification, operational qualification, and performance qualification), execution of the protocol, preparation of a summary report, and on-going validation (and revalidation if changes are made). 

Adherence to basic principles of GLP to ensure quality of the study including a detailed protocol prepared prospectively. 

Samples Catalyzed with Sodium Methoxide in Methanol Alternate Protocol Preparation of Fatty Acid Methyl Esters from Lipid DT.2.4... 

Support Protocol Preparation and Standardization of Sodium Thiosulfate... 

Support Protocol Preparation of Samples for HPLC of Organic Acids G2.2.6... 

The steps and sequence of events required to carry out a process validation assignment are outlined in Table 8. The objective of prospective validation is to prove or demonstrate that the process will work in accordance with a validation master plan or protocol prepared for pilot-product (100 x size) trials. 

What mechanism exists for validation protocol preparation and approval ... 

URS preparation Supplier audit and evaluation Qualification protocol preparation Qualification review and reporting System access security Backup, archiving, and retrieval System operation and management Contingency/recovery planning System maintenance Calibration... 

In the total synthesis of (+)-trienomycins A and F, Smith et al. used an Evans aldol reaction technology to construct a 1,3-diol functional group8 (Scheme 2.1i). Asymmetric aldol reaction of the boron enolate of 14 with methacrolein afforded exclusively the desired xyn-diastereomer (17) in high yield. Silylation, hydrolysis using the lithium hydroperoxide protocol, preparation of Weinreb amide mediated by carbonyldiimidazole (CDI), and DIBAL-H reduction cleanly gave the aldehyde 18. Allylboration via the Brown protocol9 (see Chapter 3) then yielded a 12.5 1 mixture of diastereomers, which was purified to provide the alcohol desired (19) in 88% yield. Desilylation and acetonide formation furnished the diene 20, which contained a C9-C14 subunit of the TBS ether of (+)-trienomycinol. 

Evaluate drug substance stability, including protocol preparation, approval, and study conduct. 

Reviewing and approving the study protocols prepared by the CROs and detailing the procedures to be followed to complete the study designs. The study protocol should provide information on all aspects of the study. Commonly included items in a study protocol are listed in Table 2. 

Essential Work of Fracture and Cohesive Zone Fracture Toughness, Testing protocol prepared for ESIS TC4 by E. Clutton and revised by D.R. Moore (July 2002). 

Asymmetric tetradentate chiral SB ligands having either two different salicylaldehyde derivatives or a combination of sal and acac units are prepared by the stepwise protocol, preparing first the chiral half unit intermediate which is reacted further to give the desired asymmetric... 

Figure 54.3 shows two examples of resource allocations for protocol preparation. On the bottom, the CRO proposes a team, consisting of a project physician, project manager, statistician, CRA, medical writer and secretary, with a total cost of 39120. The top shows another proposal for the same activity, where the task of writing the protocol is assigned to a physician, who will be billed at 200/h, with a total cost of 52 000. 

EXAMPLE A Protocol preparation Project physician 260 150 39 000 Total = 39 000... 

The effective execution of the VMP is based on how precisely the man-hour requirements are calculated for each task. Use input from experienced validation and engineering personnel. Consideration should be given to the time frame for protocol preparation, review, correction, and approval. Consider the analysis involved, the test equipment, and the time frame for procurement. 

The master plan is finalized during detail engineering. The protocols prepared (IQ s, OQ s and PQ s) and the validation files started during construction. The IQ s (Installation Qualifications) are performable as construction is completing and can be completed by the constructor under supervision. The OQ s (Operational Qualifications) can be performed during the earlier parts of start-up as verification of mechanical completion. The PQ s (Process Qualifications) are performed as start-up completes and continue through the operating life of the plant. For maximum schedule... 

Preparation includes contributing to pharmacotherapy, drawing up protocols, preparing drugs (including radiopharmaceuticals), assessing the quality of preparations and supporting the administration of medicines. 

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