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Pharm Ana 1 LEC > (Finals) Pharmaceutical Analysis 1 - Finals > Flashcards

(Finals) Pharmaceutical Analysis 1 - Finals Flashcards

1
Q

the measurement of the weight of a
substance in a sample or calculations of the weight of a substance in a sample from the weight of a chemically equivalent amount of some other substances

A

Gravimetric Analysis

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2
Q

Example Assay

A

● Assay of Sodium Chloride
● Assay of Sodium Lauryl Sulfate for Sodium Sulfate Content

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3
Q

The residue after incineration of the crude drug or drug from botanical origin is the ash content.

A

Ash Content

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4
Q

It represents the inorganic salts naturally occurring to the drug and adhering to it and it also include inorganic matter that is present for the purpose of adulteration.

A

Ash Content

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5
Q

Is the residue remaining after
incineration.

A

TOTAL ASH

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5
Q

Is the part of the total ash which is
insoluble in 3 N HCl

A

ACID- INSOLUBLE ASH

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5
Q

Is the part of the total ash that is
soluble in water.

A

WATER-SOLUBLE ASH

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6
Q

Residue on ignition is the measure of the amount of residual substance not volatilized from a sample when the sample is ignited in the presence of sulfuric acid.

A

Residue on Ignition (Sulfated Ash)

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7
Q

It also determines the content of inorganic impurities in an organic substance.

A

Residue on Ignition (Sulfated Ash)

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8
Q

Sulfated ash/Sulphated ash found in
European and Japan Pharmacopeia are
considered equivalent to this test, except when noted.

A

Residue on Ignition (Sulfated Ash)

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9
Q

Examples of Residue on Ignition (Sulfated Ash)

A

● Acetazolamide
● Aspirin
● Cocaine hydrochloride
● Negligible

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10
Q

an upper residue limit of 0.1%

A

Acetazolamide

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11
Q

an upper residue limit of 0.05%. For this determination 1 to 2g samples of the official substances are usually taken.

A

Aspirin

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11
Q

500mg is taken and the residue which remains must not exceed 500 microgram which means from this drug only a negligible amount of residue may remain

A

Cocaine hydrochloride

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11
Q

a quantity not exceeding 500
microgram

A

Negligible

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12
Q

a means of determining the percentage of test material which is volatized and driven off under the conditions specified.

A

Loss on Ignition (Loss on Drying)

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13
Q

Water content of varying quantities of many official drugs in the USP/NF is either as water of crystallization/ hydration or water in the absorbed form.

A

Water Content

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14
Q

In order to ensure uniformity for these
official drugs, the USP/NF specify a limit of water content on these drugs.

A

Water Content

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15
Q

Official Methodsfor Water Content Determination

A
  1. Titrimetric Method
  2. Azeotropic Method
  3. Gravimetric Method
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16
Q
  • Method 1a (Direct)
  • Method 1b (Residual)
  • Method 1c (Coulometric)
A

Titrimetric Method

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17
Q

Also known as xylene/ toluene distillation

A

Azeotropic Method

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18
Q

Use of moisture balance

A

Gravimetric Method

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19
Q

Method 1a

A

Direct

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20
Q

Method 1b

A

Residual

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21
Q

Method 1c

A

Coulometric

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22
Q

Steps for Water Content Determination

A
  1. Karl Fischer Apparatus
  2. Azeotropic Distillation
  3. Moisture Balance
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23
Q

one of the important procedures in determination of water content of official drugs.

A

Karl Fisher electrometric titration method

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24
Q

involves the titration of the sample in
reagent methanol with the Karl Fisher
reagent which consist of iodine, sulfur
dioxide, pyridine, and methanol.

A

Karl Fisher electrometric titration method

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25
Q

ADVANTAGES of Electromagnetic Titration of Water

A

● Most rapid of the official methods.
● Specific for water
● Widely applicable in determination of the water content of drug products.

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26
Q

The amount of extractives a drug or a
substance yield represents the amount of constituents or group of related constituents the sample contains.

A

Extractive and Crude Fiber Content

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27
Q

In some cases, the amount of a drug
soluble in a given solvent is a measure of purity.

A

Extractive and Crude Fiber Content

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28
Q

Volatile and Nonvolatile Ether-Soluble Extractives

A

● Total ether-soluble volatile constituents
● Nonvolatile ether-soluble constituents

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29
Q

for drugs which contain volatile oils.

A

Total ether-soluble volatile constituents

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30
Q

for drugs with volatile matter leaving
resin, coloring matter and fixed oil.

A

Nonvolatile ether-soluble constituents

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31
Q

Alcohol-SolubleExtractive

A

● Alcohol
● Method 1
● Method 2

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32
Q

good solvent for resinous matter

A

Alcohol

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33
Q

Hot extraction

A

Method 1

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34
Q

Cold extraction

A

Method 2

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35
Q

applied to drugs of which one or more of the most important constituents are soluble in water.

A

Water-SolubleExtractive and Water-Insoluble Extractive

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36
Q

Hexane-SolubleExtractive

A

● Hexane
● Hexane extractive

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36
Q

good solvent for fats and fatty oils

A

Hexane

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36
Q

the residue, consisting chiefly of cellulose, that remains undissolved after successive treatment with boiling acid and alkali.

A

Crude Fiber

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37
Q

an index in the amount of fat present
and serves as a check on the
amount of seeds contained in
colocynth pulp, since the seeds
contain a large amount of fatty
matter.

A

Hexane extractive

38
Q

The methods of analysis of fatty
substances, waxes, resins, etc., usually
consist of the determination of a number of physical and chemical properties or values commonly known as constants.

A

Constants of Fats,Fatty Oils, Waxes, Balsams, and Resins

39
Q

a.k.a. acid number and acidity index.

A

Acid Value

39
Q

the number of milligrams of potassium
hydroxide necessary to neutralize the free acid in 1g of oil, fat, wax, resin, balsam, or similar organic substances of complex composition.

A

Acid Value

40
Q

Phenolphthalein – indicator used

A

Acid Value

41
Q

a.k.a. saponification number and
Koettsdorfer number.

A

Saponification Value

42
Q

the number of milligrams of potassium
hydroxide required to neutralize the free acids and saponify the esters contained in 1g of fat, fatty or volatile oil, wax, resin, balsam, or other substances of similar composition.

A

Saponification Value

43
Q

USP Specifications: 187-193

A

Saponification Value

44
Q

important in the analysis of yellow and white wax, since it serve in many cases, to indicate the presences of adulterants, such as paraffin.

A

Ester Value

45
Q

the number of milligrams of potassium
hydroxide required to saponify the esters in 1g of a fatty or volatile oil, fat, wax, balsam, resin or similar substances.

A

Ester Value

46
Q

● Phytosterol
● Cholesterol

A

Unsaponifiable Matter

46
Q

the substances present in oils or fats that are not saponified by alkali hydroxides but are soluble in ordinary fat solvents.

A

Unsaponifiable Matter

47
Q

vegetable oils and fats

A

Phytosterol

48
Q

animal oils and fats

A

Cholesterol

48
Q

the number of grams of iodine absorbed under specified conditions by 100g of oil, fat, wax, or other substances.

A

Iodine Value

49
Q

quantitative measure of the proportion of unsaturated fatty acids present, both free and combined as esters, that have the property of absorbing iodine

A

Iodine Value

50
Q

Iodine Value oils

A
  1. Drying oils
  2. Semi-drying oils
  3. Non-drying oils
51
Q
  • > 120
  • Linseed oil
  • Fish oil
A

Drying oils

52
Q
  • 100-120
  • Cottonseed oil
  • Sesame oil
A

Semi-drying

53
Q
  • <100
  • Olive oil
  • Almond oil
A

Non-drying oils

54
Q

Methods of Determination

A

● HANUS METHOD - METHOD 1
● HANUS METHOD - METHOD 2

55
Q
  • Chloroform is used because it is soluble in organic solvent
  • Iodobromide TS is used
A

HANUS METHOD - METHOD 1

56
Q

Iodochloride TS is used

A

HANUS METHOD - METHOD 2

57
Q

a.k.a. hydroxyl number

A

Hydroxyl Value

57
Q

the number of milligrams of potassium
hydroxide equivalent to the hydroxyl content of 1g of the substance.

A

Hydroxyl Value

57
Q

the number of milligrams of potassium
hydroxide required to neutralize the acetic acid obtained by the saponification of 1g of acetylated fatty acids.

A

Acetyl Value of Fatty Acids

57
Q

gives an indication of the identity and purity of fatty substances possessing alcoholic hydroxyl groups

A

Hydroxyl Value

58
Q

certain fatty oils, particularly those of animal origin, which are not highly refined, frequently contain some moisture and non-fatty tissue residue.

A

Water and Sediment in Fatty Oils

59
Q

pear-shaped centrifuge with graduation.

A

Water and Sediment in Fatty Oils

60
Q

limit for moisture and sediment; non-
destearinated cod liver oil – NMT 0.5% by volume of water and sediment

A

Water and Sediment in Fatty Oils

60
Q

Chemical Components of Official Volatile Oils

A

● Hydrocarbon
● Alcohols
● Aldehydes
● Ketones
● Phenols
● Acids
● Sulfur compounds

60
Q

a.k.a. ethereal oils, essential oils, or
essences

A

Assay of Volatile Oils

61
Q

pinene, camphene, limonene

A

Hydrocarbon

62
Q

borneol, linalol, methol

A

Alcohols

63
Q

benzaldehyde, cinnamic aldehyde, citral

A

Aldehydes

63
Q

camphor, carvone, menthone

A

Ketones

64
Q

anethol, eugenol, thymol

A

Phenols

65
Q

propionic, butyric, bornyl acetate,
mentyl acetate

A

Acids

66
Q

allyl isothiocyanate

A

Sulfur compounds

67
Q

General Tests for Volatile Oils

A

● Specific Gravity
● Lighter than water
● Heavier than water
● Rotatory Power
● Refractive Index
● Congealing
● Temperature
● Solubility

68
Q

Specific Gravity for Volatile Oils

A

0.84 - 1.20

69
Q

Lighter than water

A

HC, Alcohols, esters, ketones

70
Q

Heavier than water

A

Aldehydes, phenol and its derivatives,
certain esters

71
Q

Refractive Index for Volatile Oils

A

1.46 and 1.61

72
Q

The esters of peppermint oil, which consist chiefly of menthyl acetate, are saponified by the alkali when the mixture is refluxed, forming free menthol and potassium acetate.

A

Assay of Ester Content(Assay of Peppermint oil for Total Esters)

73
Q

● NLT 50% of total menthol (C10H19OH)
● Uses Acetylization flask

A

Assay of Alcohol Content (Assay of Peppermint oil for Menthol)

74
Q

When no other constituents are present
which react with the reagent, the assay of aldehydes may be performed by the bisulfite method (NaHSO3).

A

Assay of Aldehyde Content (Assay of Benzaldehyde)

75
Q

Volatile oils which contain aldehyde in very small amounts, such as lemon oil, or which contain other constituents that form water-soluble addition products with sodium bisulfite cannot be assayed accurately by bisulfite method instead by the hydroxylamine method.

A

Assay of Aldehyde Content (Assay of Benzaldehyde)

75
Q

The determination is made by the bisulfite addition reaction or by the hydroxylamine method.

A

Assay of Ketone Content (Assay of Caraway Oil)

75
Q

Carvone – the principal ketone present in oil, reacts with the sodium bisulfite

A

Assay of Ketone Content (Assay of Caraway Oil)

76
Q

the principal ketone present in oil, reacts with the sodium bisulfite

A

Carvone

77
Q

Volatile oils that contain phenols when
shaken with solutions of sodium hydroxide diminished in volume because of the ready solubility of the phenol constituents in alkali; the non phenolic portion of the oil remains undissolved (cassia flask)

A

Assay of Phenol Content (Assay of Clove Oil)

78
Q

● chemical substances which are
1. obtained from plant, animal, or synthetic resources
2. contain organic nitrogen(s) within their chemical structure, and
3. usually possess physiological activity.

A

Assay of Alkaloids and Amine Drugs

79
Q

● Nitrogen(s) in alkaloids
- Amine
- nitrogen

A

Assay of Alkaloids and Amine Drugs

80
Q

Nitrogen(s) in alkaloids

A
  • Amine
  • nitrogen
81
Q

Alkaloidal Test Solutions

A

● mercuric iodide TS
● Iodine TS
● Mercuric Potassium Iodide TS

81
Q

commonly known as Valser’s reagent.

A

mercuric iodide TS

81
Q

this reagent forms white precipitate
with minute traces of many alkaloids
when added to their acidified
aqueous solutions.

A

mercuric iodide TS

82
Q

commonly known as Wagner’s
reagent.

A

Iodine TS

83
Q

yields reddish or red- brown
precipitates.

A

Iodine TS

84
Q

yields white or slightly yellow
precipitates

A

Mercuric Potassium Iodide TS

84
Q

known as Mayer’s reagent

A

Mercuric Potassium Iodide TS

85
Q

● 6-50mg/mL vial of ephedrine sulfate,
CHCl3, NaCl,
● NaOH TS
● 0.1N perchloric acid – titrant used.
● 428.56/2000
● Titer 21.43 mg
● Specs – 98-101%

A

Assay of Pharmaceutical Dosage Formsfor Alkaloidal content (official) Assay of Ephedrine Sulfate Injection (C10H15NO)2.H2SO4

86
Q

● Aminophylline – 2 mole of theophylline (C7H8N4O2)2
● 1 mole of ethylenediamine (C2H8N2)
● Standard solutions used – AgNO3 and
NH4SCN
● Titer 21.02 mg
● Specs 93-107%

A

Assay of Aminophylline Tablets (Residual Precipitation)

Pharm Ana 1 LEC (5 decks)

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