Lecture 15 - Analytical Methods Flashcards

1
Q

What does pharmaceutical analysis do?

A

determines the quality of drug products via analytical chemistry

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2
Q

What are the variety of analytical techniques?

A

spectroscopic, chromatographic and diffraction

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3
Q

What does each technique play a role in?

A

determining the quality of the pharmaceutical product and excipients

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4
Q

How to analyse pharmaceutical products?

A

UV/Vis spectroscopy

high pressure liquid chromatography

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5
Q

How to analyse the solid product?

A

Infrared spectroscopy

xray diffraction

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6
Q

UV/Vis spectrum?

A

radiate a UV light source through the sample, molecules absorb different wavelengths of radiation and the light which isn’t absorbed reaches a detector which allows us to plot absorbance vs wavelength

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7
Q

What is the lowest energy transitions?

A

rotational

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8
Q

What radiation induces transitions within rotational energy levels?

A

microwave raidation

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9
Q

What induces transitions within the vibrational energy levels?

A

Infrared radiation

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10
Q

What induces transitions within the electronic energy levels?

A

UV/Vis wavelengths

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11
Q

What are transitions?

A

electrons jumping from low energy states to high energy states

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12
Q

What else is related to electronic?

A

fluorescence and phosphorescence - related to changes in electronic structure

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13
Q

At room temp, what states are most molecules in?

A

ground vibrational and electronic states

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14
Q

How do molecules absorb radiation?

A

if polychromatic light of the correct wavelength interacts with the molecules

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15
Q

What happens to certain types of electrons?

A

they will be excited to higher energy states (electron transition)

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16
Q

What is the excitation accompanied by?

A

invariably accompanied by an increase in the energy levels of rotational and vibrational states

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17
Q

Where can transitions occur between?

A

between low electron energy levels to higher electron energy levels

can also get transitions from within the rotational energy levels, e.g. from first rotational level in the lower state to first in the higher state

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18
Q

What type of electronic transitions do not follow the specific pattern?

A

one that goes from the highest rotational energy level on the lower level, to the first rotational energy level on the higher level

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19
Q

How does a conventional spectrophotometer work?

A

polychromatic light source hits a diffraction grate, which splits the light up into its individual wavelengths (spectrum)

the exit slit then selects particular wavelengths of light that have come off the diffraction grate and allow it to pass through our sample

the sample absorbs some of the light and what isnt absorbed passes through to the PMT, which amplifies the signal

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20
Q

What is the PMT?

A

photomultiplier tube

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21
Q

How does a PDA spectrophotometer work?

A

polychromatic light passes through the whoe sample and the light is absorbed by the molecules contained

the light which is not absorbed passes through the diffraction grating, which seperates out the polychromatic light into a spectra

we then have a photodiode array which is a series of photosensitive diodes and each wavelength of light hits a specific diode

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22
Q

Benefits of PDA spectrophotometer?

A

increases the speed of analysis and allows us to asses the effect of interfering peaks more accurately

they are more expensive and have few moving components

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23
Q

Disadvantages of conventional spectrophotometer?

A

require more maintenance because they have many moving components

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24
Q

What is beer’s law?

A

the intensity of a beam of parallel monochromatic light decreases exponentially with the number of absorbing molecules

absorbance is proportional to the concentration

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25
What does lambert's law state?
absorbance is proportional to path length
26
What is the beer lambert law?
A = A(1%, 1 cm).b.c
27
what is the A11 value?
the specific absorbance or specific absorbance coefficient
28
What is c in BL?
concentration in g/100ml (%w/v)
29
what is A in BL?
absorbance
30
what is b in BL?
path length in cm
31
What is A(1%, 1 cm)?
the absorbance of a 1g/100ml solution in a 1cm cell at a specific wavelength
32
What does light scattering in a sample cause?
absorbance > true, we overestimate the absorbance
33
What is light scattering?
the light will hit small particles in the sample, and will be scattered, hitting internal surfaces of the UV spectrophotometer the light is no longer making it to the detector and the detector things its been lost
34
How can we prevent light scattering?
by filtering our sample
35
What can the beer lambert law quantify?
the amount of sample present or the amount of analyte in a sample
36
What does ionisation cause?
structural changes that can cause changes in the electronic system, this changes the UV spectra it causes a shift in the absorption spectra
37
What is an issue with UV/Vis?
its lack of specificity it does not allow us to discriminate between closely related structures
38
What is absorbance?
additive, so total absorbance may be from more than one compound absorbing at that particular wavelength
39
What is chromatography?
a separation technique
40
How does chromatography work?
we spot our mixture of component on the TLC plate of an appropriate solvent, and immerse this within the tank the bottom of the TLC plate sits within the mobile phase and through capillary action it would be drawn up the plate as the mobile phase migrates up the plate, it drags along the components at different rates
41
What affects the rate the components are separated at?
the interaction with the stationary phase if it interacts more strongly with the stationary phase, it will be more retained
42
What is column chromatograpy?
mixture is applied to the column in solvent applying a flow of eluate to this compound allows the components to start to migrate through the column
43
what is the stationary phase typically in chromatography?
silica gel
44
What does column chromatography allow us to get?
a chromatogram, plotting response against time
45
What does the chromatogram allow?
to quantify the use of the components within the mixture
46
What is the frequency of use of tablets and capsules?
``` tabs = 46% capsules = 13% ```
47
What is the frequency of use of oral liquids and injections?
oral liquids = 16% | injections = 15%
48
What are the physiochemical properties of solid dosage forms correlated to?
the crystal structure of the raw materials
49
What does the final product affect?
the stability and the bioavailability
50
What is an IR spectrum?
graph of absorbance or % transmission against wavelength or wavenumber %T = It/Io and A = log Io/It
51
What is the wavenumber?
number of waves in 1cm units are cm-1
52
What is energy of IR proportional to?
E = 1/wavelength
53
IR has less energy than..?
UV/visible light
54
What does absorption of IR cause transitions in?
vibrational and rotational energy levels
55
For a compound to be active in IR what must absorption cause?
a change in dipole moment of the molecule
56
Stretching vibrations?
symmetric and asymmetric result in a shift in the dipole of the molecule
57
Bending vibrations?
in plane rocking in plane scissoring out of plane wagging out of plane twisting
58
What do bending vibrations result in?
A change of the dipole moment of the molecule
59
What is a strength of IR?
The specificity
60
What is the lower region of the IR spectrum?
the finger print region specific to each individual molecule
61
What can we use the finger print region for?
to determine the exact structure of our analyte
62
What is polymorphism?
the ability of a compound to crystallise in more than one 3D packing arrangement
63
What do different polymorphs have?
distinct IR patterns if we look at the finger print regions
64
What can polymorphism cause?
different dissolution and bioavailability
65
What is the unit cell of a molecule?
the smallest repeating unit
66
What is Bragg's law?
nλ = 2dsinθ
67
What do crystalline forms show?
diffraction
68
What do amorphous forms show?
they do not diffract
69
What types of X ray diffraction are available?
powder or single crystal X ray diffraction
70
What does powder X ray diffraction give us?
a similar finger print pattern as IR
71
what does single crystal X ray diffraction give?
absolute structure of particular analyte