TOPIC 3: Data Quality

Question 1

A deviation from the absolute value or from the true average of a large number of results.

Answer 1

Error

Question 2

Error can be classified as?

Answer 2

systematic error and indeterminate error

Question 3

Classes of Error

Answer 3

Systematic (Determinate Errors)
Random (Indeterminate Errors)

Question 4

Errors that are reproducible and can be discovered and corrected.

Answer 4

Systematic Errors

Question 5

Systematic Errors can be further classified into:

Answer 5

Instrumental Error
Method Error
Personal Error

Question 6

Failure to calibrate, degradation of parts in the instrument, power fluctuations, variation in temperature.

Answer 6

Instrumental Errors

Question 7

Errors due to no ideal physical or chemical behaviour, completeness and speed of
reaction, interfering side reactions, sampling problems.

Answer 7

Method Errors

Question 8

Occur where measurements require judgment, result from prejudice, color acuity problems, negligence to follow proper procedures.

Answer 8

Personal Errors

Question 9

This is observed by the same analyst when the successive measurements are made with the SAME IDENTICAL conditions.

Answer 9

Random Errors

Question 10

Determinate Errors

Answer 10

Systematic Errors

Question 11

Indeterminate Errors

Answer 11

Random Errors

Question 12

Appear as slight variations in successive measurements due to causes that the analyst can not control.

Answer 12

Random Errors

Question 13

A plot of indeterminate error would show a ________ frequency curve.

Answer 13

normal

Question 14

This is establishing documented evidence which provides a high degree of assurance that a specific process, method, system, activity or equipment consistently produce a product meeting its predetermined specifications.

Answer 14

Validation

Question 15

Pertains to agreement of an experimental results with true value.

Answer 15

Accuracy

Question 16

The measure of reproducibility of data within a series of results

Answer 16

Precision

Question 17

Measure of central tendency.

Answer 17

Mean

Question 18

Difference between largest/smallest observations in a set of data.

Answer 18

Range

Question 19

This measures the difference of the actual values with the mean value.

Answer 19

Average Deviation

Question 20

Determined by dividing the average deviation by the mean.

Answer 20

Relative Average Deviation

Question 21

Sum of squares difference of the actual values with the mean value/total number of samples.

Answer 21

Variance

Question 22

Square root of variance

Answer 22

Standard Deviation

Question 23

____________ of an analytical procedure is the process by which it is established, by laboratory studies, that the performance characteristics of the procedure meet the requirements for the intended analytical applications.

Answer 23

Validation

Question 24

This provides an assurance of reliability during normal use, and is sometime referred to as “the process for providing documented evidence that the method does what it is intended to do.”

Answer 24

Method Validation

Question 25

Purpose of Validation

Answer 25

For identification of sources and quantitation of potential error

To determine if method is acceptable for intended use.

To satisfy FDA requirements

To ensure the consistency of the output

Question 26

TYPES OF ANALYTICAL PROCEDURES TO BE VALIDATED

Answer 26

1. Identification tests
2. Quantitative tests for impurities content.
3. Limit tests for the control of impurities
4. Quantitative tests of the active moiety in samples of drug substance.

Question 27

Validation Parameters

Answer 27

Accuracy

Precision

Range

Specificity

Linearity

Ruggedness

Question 28

The closeness of test results obtained by that procedure to the true value.

Answer 28

Accuracy of an analytical procedure

Question 29

Determined by application of the analytical procedure to an analyte of known purity (e.g. A Reference Standard).

Answer 29

Accuracy

Question 30

Accuracy should be assessed using ___________________________, covering the specified range. (i.e. Three concentrations and three replicates of each concentration

Answer 30

a maximum of 9 determinations over a minimum of 3 concentration levels

Question 31

It is the degree of agreement among individual test results when the procedure is applied repeatedly to multiple samplings of homogeneous sample.

Answer 31

Precision

Question 32

Precision may be a measure of either the degree of ____________ or of ____________ of the analytical procedure under normal operating conditions.

Answer 32

reproducibility or repeatability

Question 33

Expresses the precision under the same operating conditions over a short interval of time.

Answer 33

Repeatability

Question 34

Repeatability is also termed ?

Answer 34

intra-assay precision

Question 35

Expresses variations within laboratories, such as different days, different analysts, different equipment, and so forth.

Answer 35

Intermediate precision

Question 36

In intermediate precision, to verify that in the same laboratory the method will provide the _____________ once the development phase is over.

Answer 36

same results

Question 37

Expresses the precision between laboratories. The objective of reproducibility is to verify that the method will provide the same laboratories results in different laboratories.

Answer 37

Reproducibility

Question 38

The ability to measure accurately and specifically the analyte of interest in the presence of other components that may be expected to be present in the sample matrix.

Answer 38

Specifity

Question 39

In case of identification tests, the method should be able to discriminate between compounds of closely related structures which are likely to be present.

Answer 39

Specificity

Question 40

It is the lowest amount of analyte in a sample that can be detected, but not necessarily quantitated, under the stated experimental conditions.

Answer 40

Detection Limit

Question 41

The detection limit is a characteristic of?

Answer 41

Limit tests

Question 42

Detection Limit is usually expressed as the ___________________ (e.g., percentage, parts per billion) in the sample.

Answer 42

concentration of analyte

Question 43

It is the lowest amount of analyte in a sample that can be determined with acceptable precision and accuracy under the stated experimental conditions.

Answer 43

Quantitation Limit

Question 44

A characteristic of quantitative assays for low levels of compounds in sample matrices, such as impurities in bulk drug substances and degradation products in finished pharmaceuticals.

Answer 44

Quantitation Limit

Question 45

Its ability to elicit test results that are directly, or by a well-defined mathematical transformation, proportional to the concentration of analyte in samples within a given range.

Answer 45

Linearity

Question 46

It refers to the linearity of the relationship of concentration and assay measurement.

Answer 46

Linearity

Question 47

Requires a minimum of 5 concentration levels.

Answer 47

Linearity

Question 48

it is the interval from the upper to the lower concentration (amounts) of analyte in the sample for which it has been demonstrated that the analytical procedure has a suitable level of precision, accuracy and linearity.

Answer 48

Range

Question 49

It’s the measure of its capacity to remain unaffected by small but deliberate variations in procedural parameters listed in the procedure documentation and provides an indication of its suitability during normal usage.

Answer 49

Robustness

Question 50

Refers to the degree of reproducibility of test results under a variety of conditions such as:

Different laboratories

Different Analysts

Different Instruments

Different Davs

Answer 50

Ruggedness

Question 51

Ruggedness refers to the degree of reproducibility of test results under a variety of conditions such as:

Answer 51

Different laboratories
Different Analysts
Different Instruments
Different Davs

Question 52

Data Elements Required for Validation

Answer 52

Category I: Analytical methods for quantitation of major components of bulk drug substances

Category II: Analytical methods for determination of impurities in bulk drug substances

Category III: Analytical methods for determination of performance characteristics

Category IV: Identification tests.