Mdcm 605-Final

Front 1

Which one of the 3 types of quantitative analysis errors is the following:

easy to recognize since they involve a major breakdown in the analytical process, such as samples being spilt, wrong dilutions being prepared, or instruments breaking down or being used in the wrong way.

Back 1

Gross Error

Front 2

Which one of the 3 types of quantitative analysis errors is the following:

characterized by precise and inaccurate measurement results.

Back 2

Systemic error

Front 3

Which one of the 3 types of quantitative analysis errors is the following:

characterized by widely scattered, i.e., imprecise, measurement results.

Back 3

Random error

Front 4

Accuracy and precision:
the calculated value for __ provides a formal expression of the scatter in the results from an analysis rather than the visual judgment shown previously.

Back 4

standard deviation

Front 5

provides an exact description of how the analysis is carried out.

Back 5

Analytical procedure

Front 6

expresses the closeness of agreement(degree of scatter) b/w a series of measurements obtained from multiple sampling of the same homogeneous sample

Back 6

precision

Front 7

precision obtained under the same operating condition over a short period of time(an assay is repeated by the same person using the same equipment)

Back 7

Accuracy

Front 8

expresses the within-laboratory variation of precision when the analysis is carried out by different analysts, on different days, and with different equipment

Back 8

intermediate precision

Front 9

expresses the precision b/w laboratories such as when a method is transferred from one part of a company to another.

Back 9

reproducibility

Front 10

simplest method is to compare a substance being analysed with a reference standard analysed by the same procedure (the reference standard is a highly characterized form of the drug that has been subjected to extensive analysis)

Back 10

accuracy

Front 11

relates to the performance of the analytical equipment(the four Q's)

Back 11

system suitability- these test are designed to show that the system meets the standards required by the method

Front 12

consists of all of the reagents or solvents used in an analysis without any of the analyte being present

Back 12

analytical blank

Front 13

comparison of the value or values of a particular parameter measured by the system under strictly defined conditions with the preset standard values

Back 13

calibration

Front 14

the smallest amt of an analyte which can be detected by a particular method.

Back 14

limit of detection

Front 15

smallest amount of analyte which can be quantified reliably

Back 15

limit of qualification

Front 16

most analytical methods are based on processes where the method produces a response that is linear and which increases or decreases linearly with analyte concentration

Back 16

linearity

Front 17

refers to the interval between the upper and lower concentration of an analyte for which an acceptable level of precision and accuracy has been established

Back 17

range

Front 18

evaluated to determine how resistant the precision and accuracy of an assay are to small variations in the method (for example, the stability of analytical solutions, or the length of sample extraction time)

Back 18

robustness

Front 19

measure of how capable a method is of measuring the analyte alone in the presence of other compounds contained in the sample

Back 19

selectivity

Front 20

indicates how responsive the method is to a small change in the concentration of an analyte (may be viewed as the slope of a linear response curve)

Back 20

sensitivity

Front 21

indicates how responsive the method is to a small change in the concentration of an analyte (may be viewed as the slope of a linear response curve)

Back 21

weighing by difference

Front 22

often encountered in relation to the composition of mobile phases used in high-pressure liquid chromatography (for example, when 30 ml methanol is mixed with 70 ml water, a 30:70 v/v mixture is formed)

Back 22

v/v

Front 23

usually used to express the content of an active ingredient in liquid formulations such as injections, infusions, and eyedrops

Back 23

w/v

Front 24

a common measure used to express the concentration of active ingredient in a formulation such as a cream

Back 24

w/w

Front 25

common measure used for impurities in drug substances, particularly heavy metals and solvents

Back 25

ppm

Front 26

physical properties of drug molecules, such as ________________
__________, along with simple chemical ___________ and degradation reactions, play an important part in the design of analytical methods

Back 26

pKa + partition coefficient
derivitization

Front 27

what is the most effective range for a buffer

Back 27

1 pH unit either side of the pKa value of the weak acid or base used in the buffer

Front 28

the partition coefficient for a compound (P) can be simply defined as ________ where Cois the concentration of substance in an organic phase and Cwis the concentration of substance in water

Back 28

P=Co/Cw

Front 29

the ________ the more a substance has an affinity for organic media

Back 29

Greater the P

Front 30

in zero-order kinetics the rate of degradation is WHAT in regards to reactant concentration?

Back 30

Independent of the concentration of the reactants.

Front 31

1st order degradation has what typical degradation pattern?

Back 31

The hydrolysis of a drug in solution

Front 32

The lack of what about the double bond ensures that the stereochemistry of a drug and its isomer are different?

Back 32

lack of free rotation

Front 33

when is a compound said to be chiral

Back 33

when there is no symmetry around carbon

Front 34

when __ is present in a moecule, there is a possibility of diastereomers

Back 34

more than one chiral center

Front 35

analytical derivitization is employed for two reasons:
to improve the analysis by improving the __
and
to improve the analysis by improving chromatographic behavior of detectability, i.e. __

Back 35

selectivity
sensitivity

Front 36

Ultraviolet and Visible Spectroscopy:

radiation in the wavelength range _________________ is passed through a solution of drug

Back 36

200 to 700nm

Front 37

most drug molecules absorb radiation in the ultraviolet region of the spectrum, i.e., ___________

Back 37

100 to 350nm

Front 38

short wavelength UV radiation ________ can cause the strongest bonds in organic molecules to break
–
weaker bonds in molecules are of more interest to the analyst because they can be excited by longer wavelength UV radiation __ _______ which is at a longer wavelength than the region in which air (for example, oxygen and carbon dioxide) and common solvents absorb

Back 38

<150nm
200nm

Front 39

chemical substructures that are responsible for the absorption of electromagnetic radiation are called ______________(1)
–a most common ___________(1) in drug molecules is the ________
__________________________(2)

Back 39

(1) chromophores
(2) aromatic ring, such as the benzene ring

Front 40

the___________ by a solution of molecules is governed by the Beer-Lambert Law

Back 40

measurement of light absorption

Front 41

–
in pharmaceutical products, concentrations and amounts are usually expressed in grams or milligrams, and, for the purposes of analysis of these products, the Beer-Lambert equation is written in the following form, _________________

Back 41

A=A(1%,1cm)bc

Front 42

Ultraviolet and Visible Spectroscopy:

the __________, a deuterium lamp for the UV region from 190 to 350 nM and a quartz halogen or tungsten lamp for the visible region from 350 to 900 NM

Back 42

light source

Front 43

since measurements are usually made in a 1 cm cell, the equation can be written as _________________ which gives the concentration of the analyte in g/100 ml

Back 43

c=(a/A(1%, 1cm)

Front 44

the ______________, used to disperse the light into its constituent wavelengths

Back 44

monochromator

Front 45

the _____, may be designed to split the light beam so that the beam passes through two sample compartments, and, in such a double beam instrument, a blanksolution can then be used in one compartment to correct the reading or spectrum of the sample

Back 45

optics

Front 46

____ are generated in a high-vacuum region, or immediately prior to a sample entering a high-vacuum region, using a variety of methods for ion production

Back 46

charged molecules of molecular fragments

Front 47

GC/MS and LC/MS provide highly sensitive and specific methods for determining drugs and their ____________________________

Back 47

metabolites in biological fluids and tissues

Front 48

which of the two is cheaper and more sensitive?

Mass spectrometer or magnetic sector instrument

Back 48

Mass spectrometer

Front 49

in this form of analysis, spectra may contain molecular ion only

Back 49

Mass spectrometry

Front 50

the most frequently used analysis technique in pharmaceutical analysis

Back 50

chromatography

Front 51

the length of time it takes a retained compound to pass through the column depends on the compounds ________________ which is a measure of the degree to which the compound partitions (adsorbs) into the stationary phase from the mobile phase

Back 51

capacity factor

Front 52

what would happen in chromatography if a compound does not partition appreciable into stationary phase.

Back 52

It will travel through the column at the same rate as the solvent

Front 53

Calculation of column efficiency
the ______ a chromatographic peak is relative to its retention time, the less efficient the column it is eluting from

Back 53

broader

Front 54

•
Calculation of column efficiency
– the efficiency of the column is most readily assessed from the width of the peak at its height W1/2 and its retention time using the following formula, n= 5.54(tr/W1/2)2
– where, nis the number of _______________, where, tris the time taken for the compound to pass through the column, where, W1/2is the width of the peak at half its height
– _______________ is usually expressed in theoretical plates per meter, or nx (100 cm/m)/L
– where, Lis the column length in cm

Back 54

theoretical plates
column efficiency

Front 55

•Stationary and mobile phases
–there are two principal mechanisms which produce retention of a compound passing through an HPLC column
–silica gel, a ___________ column packing, where the mechanism of retaining a compound is by ____________________ onto the polar groups of the stationary phase
–octadecylsilane-coated (ODS-coated) silica gel, a ____________column packing, where the mechanism of retaining a compound is due to _______into the stationary phase.

Back 55

-Normal-phase
-adsorption of the polar groups of a molecule
-reverse plase
-partitioning of the lipophilic portion of a molecule

Front 56

High-pressure liquid chromatography (HPLC)

•Structural factors which govern the rate of elution of compounds from HPLC columns –neutral compounds

–for a neutral compounds it is the balance between its __________
__________ which will determine the time it takes to elute from an HPLC column

–the pH of the mobile phase does not play a part

–in the case of a reverse-phase column (ODS-coated silica gel), the _____________ a compound is the more it will be retained

–in the case of a normal-phase column (silica gel), the _________ a compound is the more it will be retained

–polarity can often be related to the number and strength of hydrogen-bonding functional groups in a molecule

Back 56

-polarity and lipophilicity
-more lipophilic
-more polar

Front 57

HPLC:

–
the control of the rate of elution via control of the pH of the mobile phase is only applicable to compounds in which the _____________________ (the majority of common drugs)

Back 57

degree of ionization is dependent on pH

Front 58

reverse-phase chromatography increases the

Back 58

retention time

Front 59

•Summary of detectors used in HPLC

–for the majority of analyses of drugs in formulations, variable wavelength ___________ are used which are based on the absorption of UV light by an analyte

–the diode array detector ( UVDAD) is an advanced type of UV detector with the ability to monitor across the full UV range simultaneously

–________________________ (ELSD) which is based on the scattering of a beam of light by particles of compound remaining after evaporation of the mobile phase

Back 59

-UV detectors
-Evaporative light scattering detector