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PH 105 > Special Methods in Pharmaceutical Analysis > Flashcards

Special Methods in Pharmaceutical Analysis Flashcards

1
Q

Employed in the determination of ash, moisture, crude fiber, extractives, estimation of alkaloidal content

A

Chemical Methods

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2
Q

those in which the effects of drugs upon microbes, animals, or animal
tissues are measured and which are employed in the absence of satisfactory
chemical methods for standardization

A

Biological Methods

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3
Q

Assay of drugs that use biologicals (such as animals) to determine their effect

A

Bioassays

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4
Q

What are some biological methods?

A

Bioassays
Microbiological Assays

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5
Q

Enumerate some commonly used bioassay

A

Corticotropin (rats)
Digitalis (pigeon)
Heparin (sheep)
Insulin (rabbits)
Oxytocin (chicken)
Parathyroid (dog)

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6
Q

Enumerate commonly used Microbiological Assays

A

Antibiotics
Vitamin B12

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7
Q

Determination of the ___ ________ of a crude drug which is a
representative of the inorganic salts that are either naturally
occurring in the drug or added as impurity for the purpose of
adulteration.

A

Ash Content

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8
Q

is generally taken to be the residue remaining after incineration

A

Ash Content

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9
Q

It is the residue remaining after incineration at 675±25°C

A

Total Ash

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10
Q

500°C to 550°C

A

Very Dull-Red

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11
Q

550°C-700°C

A

Dull-Red

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12
Q

800°C-1000°C

A

Bright Red

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13
Q

1000°C-1200°C

A

Yellow Red

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14
Q

1200°C to 1600°C

A

White

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15
Q

Part of the total ash which is insoluble in diluted HCl

A

Acid-Insoluble Ash

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16
Q

Formula for Acid-Insoluble ash

A

%AIA = wt of residue/wt of Sample (100)

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17
Q

Part of the total ash which represents soluble chlorides, alkali and
NH4 salts at 450°C.

A

Water-Soluble Ash

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18
Q

What are the sample, access to air, and what is left to the ash content technique ignition

A

Sample - inorganic
Access to Air - Yes
WHAT is left? - residue

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19
Q

What are the sample, access to air, and what is left to the ash content technique incineration

A

Sample - Organic
Access to Air - yes
WHAT is left? - Ash

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20
Q

What are the sample, access to air, and what is left to the ash content technique carbonization

A

Sample - Organic
Access to Air - No
WHAT is left? - charcoal

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21
Q

it dissolves the calcium carbonate, alkali chlorides, etc., leaving an acidinsoluble residue that consists almost entirely of silica derived from the soil adhering to the drug

A

Diluted hydrochloric acid

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22
Q

The ash content of chemicals is determined by ignition to dull
redness

A

Residue on Ignition

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23
Q

What are the applications of residue on ignition

A

Applications:
Ø It is necessary to control the amount of inorganic matter (adulteration) in substances (especially those that are intended for hypodermic administration)
ØStandard requirement (for inorganic matter): NEGLIGIBLE amount

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24
Q

Determines the percentage of test material that is volatilized and
driven off under the conditions specified.

A

Loss on ignition

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25
The procedure is nondestructive to the substance under test; however, the substance may be converted to another form such as anhydride.
Loss on ignition
26
What are the procedures in the loss on ignition?
1. Weigh the specime 2. Transfer to the tared crucible an accurately weighed quantity 3. Conduct the ignition 4. Ignite for successive 1-hour periods 5. Weigh the residue on ignition
27
Determination of the amount of water in an amount of sample
Water content
28
Water adsorped on the surface of the solid
Free/Unbound Water
29
water of crystallization/water of hydration
Bound water
30
in water content it has impurities
Free/Unbound Water
31
part of the crystal structure of the substance
Diluent
32
What are the applications of Water Contnent
Applications: Ø When crude drugs are sold with a guaranteed assay for active constituent, the %active constituent must be calculated on a dried-basis (moisture-free) as moisture adversely affect the calculated results. Ø Moisture promotes microbial growth (therefore, must be determined and minimized in sample of drugs)
33
What are some water Determination methods?
Method 1: Titrimetric Method (Karl Fisher Method) Method II: Azeotropic (Toluene Distillation) Method Method III: Gravimetric Methods
34
also known as Karl Fisher Methods
Titrimetric Methods
35
This method is the most rapid of the official methods, requires only small sample, is specific for water, and is widely applicable in determination of the water content of drug products.
Karl Fischer Method
36
Involves the titration of sample in reagent methanol with the Karl Fischer reagent, which consists of:
- Iodine (OA) - Sulfur Dioxide (RA) - Pyridine (base) - Methanol (solvent)
37
What is the Karl Fisher Reagent:
1mL = 5 mg of water
38
What is the Primary standard, secondary standard, endpoint and titer value of Karl Fischer Method
Primary Standard: Sodium Tartrate Secondary Standard: Water-methanol solution Endpoint: Canary-yellow to amber color Each mg of sodium tarttrate is equivalent to 0.1566 mg of water
39
Endpoint is determined by the slight excess of Karl Fischer Reagent (KFR) in the solution, canary-yellow to amber.
Direct Titration of Karl Fischer Method
40
An excess of Karl Fischer Reagent is added to the solution and the excess is backtitrated with a standard solution of water in methanol
Residual Titration of Karl Fischer Method
41
Amount of water is computed from the amount of electricity that was produced, 10.71C is equal to 10 mg of water
Coulometric Titration of Karl Fischer Method
42
What is Azeotropic-Toluene Distillation also known as?
Also known as Xylene Method, Azeotropic Method (USP); Moisture Method by Toluene Distillation (NF)
43
Water and Toluene forms what?
Azeotrope
44
Based on the loss of weight of the sample after drying or the gain in weight of the desiccant
Gravimetric Methods
45
WHAT is Acid Value also known as?
Acid Index Acid Number
46
The number of milligrams of KOH (or NAOH) necessary to neutralize the free acids in 1 g of a substance (oil, fat, wax, resin, balsam, or similar organic substance of complex composition).
Acid Value
47
What are the causes of free acids?
Hydrolysis by chemical treatment Bacterial Action Catalytic Action of heat and light
48
Does fresh or recently prepared fatt substances contain free acids?
No or Little of it
49
Upon _____, acid value increases
aging
50
High Acid values are not necessarily an indication of _________.
rancidity
51
The number of milligrams of KOH required to saponify the esters contained in 1g of substance (fat, fatty or volatile oil, wax, resin, balsam or other substance of similar composition)
Ester value
52
For substances that do not contain free acids, the ester number is _____ to saponification number. This is also the difference between the acid and saponification value
equal
53
What is ester value analyzing what?
Analysis of yellow and white wax
54
Saponification Value is also known as?
Saponification Number or Koettsdorfer Number
55
The number of milligrams of KOH required to neutralize the free acids and saponify the esters contained in 1g of substance (fat, fatty or volatile oil, wax, resin, balsam or other substance of similar composition).
Saponification Value
56
The substances present in oils or fats that are not saponified by alkali hydroxides but are soluble in ordinary fat solvents.
Unsaponifiable number
57
The number of milligrams of KOH equivalent to the hydroxyl content of 1g of the substance.
Hydroxyl Value
58
Gives an indication of the identity and purity of fatty substances possessing alcoholic hydroxyl groups.
Hydroxyl Value
59
What does low value mean in hydroxyl value?
Low Value
60
The number of grams of iodine absorbed under specified conditions by 100 g of a substance (oil, fat, wax or other substance)
Iodine Value
61
Quantitative measure of the proportion of unsaturated fatty acids present, both free and combined as esters, that have the property of absorbing iodine.
Iodine Value
62
A measure of the degree of saturation of the sample
Iodine Value
63
Based on the ability of the double bonds to absorb iodine, the xs I2 is backtitrated with 0.1 N Na2S2O3
Iodine Value/Iodometry
64
High iodine Value (above 120)
Drying oils
65
Low iodine Value (below 100)
Non drying oils
66
between 100 to 120
Semidrying oils
67
usually less than 90
Animal Fats
68
Examples of drying oils
Linseed oil Co-liver oil
69
Example of nondrying oils
Olive oil Almond oil
70
examples of semidrying oils
cottonseed oil sesame oil
71
What are the methods for determining iodine value?
Hubl Hanus Wijs
72
Iodine in Mercuric Chloride
Hubl
73
Iodine in Bromine Solution (forming IBr in glacial acetic acid)
Hanus
74
Iodine in CCl4 (forming ICl in glacial acetic acid)
Wijs
75
Found by acetylating hydroxyl fatty acids and determining the saponification value of the substance.
Acetyl Value
76
The number of milligrams of KOH required to neutralize the acetic acid obtained by the saponification of 1g of acetylated fatty acids.
Acetyl value
77
What is volatile oils also known as?
Ethereal oils or essential oils or essences
78
Types of Volatile oils
Hydrocarbons Alcohols Aldehydes Ketones Phenols Acids Sulfur compounds
79
Residual Alkalimetry with reflux
Ester content
80
what example is used for ester content
Peppermint oil for total ester
81
Reaction with acetic anhydride
Alcohol contet
82
what is the example used in alcohol content
Peppermint oil for total menthol
83
What are the processes involved in Aldehydes and ketone?
Bisulfite additon Hydroxyl amine HCl

PH 105 (6 decks)

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