Quality control sampling activities

The analysis of quality control samples is an important activity for laboratories and to make the most of the data, control charts should be used. This chapter has discussed a number of common types of control chart and described how they are set up and interpreted. 

Each laboratory should have a quality assurance program which should be well understood and used by individuals as well as by laboratory organizations to prevent, detect, and correct problems. The purpose is to ensure that the results have a high probability of being of acceptable quality. Ongoing activities may include preventative instrument maintenance, performance verification and calibration, system suitability testing, analysis of blanks and quality control samples, and ensuring system security. A plan should be set up to... 

A solvent free, fast and environmentally friendly near infrared-based methodology was developed for the determination and quality control of 11 pesticides in commercially available formulations. This methodology was based on the direct measurement of the diffuse reflectance spectra of solid samples inside glass vials and a multivariate calibration model to determine the active principle concentration in agrochemicals. The proposed PLS model was made using 11 known commercial and 22 doped samples (11 under and 11 over dosed) for calibration and 22 different formulations as the validation set. For Buprofezin, Chlorsulfuron, Cyromazine, Daminozide, Diuron and Iprodione determination, the information in the spectral range between 1618 and 2630 nm of the reflectance spectra was employed. On the other hand, for Bensulfuron, Fenoxycarb, Metalaxyl, Procymidone and Tricyclazole determination, the first order derivative spectra in the range between 1618 and 2630 nm was used. In both cases, a linear remove correction was applied. Mean accuracy errors between 0.5 and 3.1% were obtained for the validation set. 

In the Phadebas TM amylase test (72) (Pharmacia Labs) the substrate was a water insoluble cross-TTnked blue starch in tablet form which also contains some inert ingredients, sodium and potassium phosphate buffer salts and sodium chloride. This polymer was hydrolyzed by amylase into water soluble blue starch fragments. After centrifugation the absorbance of the blue supernatant was proportional to the activity of amylase present in the test samples. The day to day variation on a quality control serum had a coefficient of variation of 2.7% based on 30 days of data in our laboratory. The method is simple, reproducible and uses microquantities of serum. 

In many pharmaceutical companies, quality control departments already use NIRS to identify formulations. Figure 23 illustrates a PLS calibration for the active content determination in a low-dose tablet. Once identity testing is passed, it is straightforward to consider as a next step the determination of active content in intact tablets. Thus, qualitative and quantitative analysis can be performed by acquiring a single NIR spectrum per sample. Two analytical techniques are replaced by one—nondestructive—NIR measurement. For this purpose near-infrared spectroscopy is a fast and powerful alternative to traditional analysis, which only remains necessary as reference analytics. 

Biotinidase has not been included in external quality control programs, and no control samples are commercially available. Assessment of quality is performed by including a plasma sample of an individual with normal biotinidase activity in each assay set. Such a sample is ideally stored at - 70°C in aliquots and thawed just once (see Pitfalls and Limitations , below). 

Sample quality is generally assessed by the determination of /J-galactosidase activity. For MPS type IVB, the a-mannosidase activity is chosen as an indicator enzyme. Leukocyte homogenates that are sufficient for at least 20 separate runs are prepared from one source and aliquots are kept frozen. These samples serve as quality controls for each run. Heat-inactivated leukocyte homogenates may serve as a positive control (patient-mimics). 

Receipts of active ingredient raw materials B1 and B2 are accepted by quality control based on standard tests for potency, chemical attributes, and particle size. Particle size is determined by sieve analysis. Unfortunately, this is a limit test in which 99% of the sample must pass through a certain mesh screen, therefore any influence particle size distribution might have on dosage form potency cannot be examined. 

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