PHARMACEUTICAL CHEMISTRY 1

LABORATORY
Grace Marie C. Alunan, RPh, CPS, MSc

INORGANIC PHARMACEUTICAL
MEDICINALS

INORGANIC PHARMACEUTICAL
MEDICINALS
Normal Healthy Intestine

Continuous exchange of water through the intestinal wall by

osmosis

Upto 20L of water is

Secreted and nearly as much is reabsorbed every 24 hours

Mechanism allows reabsorption into the blood stream of

soluble metabolites from digested food

INORGANIC PHARMACEUTICAL
MEDICINALS
In State of Diarrhea

There should be electrolyte ion balance

More water is secreted than reabsorbed

Sodium is also lost (stored in the intersititial fluid and blood plasma
extarcellular fluids)

Chronic loss of K (repeated attacks of diarrhea) (K held in the

intercellular fluids), results in muscular weakness, lethargy and anorexia.

INORGANIC PHARMACEUTICAL
MEDICINALS

Concentration of Sodium

In the extracellular fluid - 135 - 150 mmol/L for proper

functioning of the body

Controlled by the renal function

INORGANIC PHARMACEUTICAL
MEDICINALS
In Case of Dehydration

Water is conserved by anuria (nonpassage of urine), in practice is defined as

passage of less than 50mL of urine in a day. Anuria is often caused by failure in
the function of the kidneys

Sodium is not regulated

Continued Diarrhea

Cause rapid depletion of water and sodium

More than 10% loss of body fluids, death may occur

INORGANIC PHARMACEUTICAL
MEDICINALS
Oral Rehydration Salt
Best method to combat dehydration caused by diarrhea

50mL/kg body weight (for mild dehydration)

100mL/kg given over 4 hours (moderate dehydration)

INORGANIC PHARMACEUTICAL
MEDICINALS
Procedure

Prepare for 100mL ORS

AMOUNT FOR 1L

NaCl

3.5g

NaHCO

2.5g

KCl

1.5g

CHO

20g

AMOUNT FOR
100ML

Dissolve the components in distilled water to prepare for

100 mL ORS

INORGANIC PHARMACEUTICAL
MEDICINALS
Properties:

Describe the color, odor, and taste of the solution formed

Calculate the total amount of Na (from NaHCO & NaCl), K

(from KCl), total Cl (from NaCl & KCl), HCO (from NaHCO )
and glucose (CHO) express in mmol/L present in the
prepared solution

INORGANIC PHARMACEUTICAL
MEDICINALS
Preparation of Precipitated Sulfur

CaO + HO Ca(OH)
Ca(OH) + S CaS + CaSO + HO
CaS + HCl S + CaCl + HS
Properties
A. Physical Properties
1. Observe the color, odor and form of sulfur prepared:
2. Pinch amount of S + 1mL distilled water reaction with litmus

INORGANIC PHARMACEUTICAL
MEDICINALS
B. Test of Purity
1. 15 mL washing divided into 3 portion
1st portion - reaction with litmus paper
2nd portion - + 2 mL KCO
3rd portion - + 2mL AgNO
Described result & note the impurities tested for
2. Pinch amount of Precipitated Sulfur + 1 mL CS. Note the solubility

INORGANIC PHARMACEUTICAL
MEDICINALS
Preparation of Boric Acid

NaBO 10HO + 2HCl 4HBO + 2NaCl + 5HO

A. Physical Properties
1. Observe: Color, odor and taste of the product
2. Described the form of HBO
3. Describe the feeling to touch: rub between the fingers a small
amount of HBO

INORGANIC PHARMACEUTICAL
MEDICINALS
B. Test for Identity
1. Pinch amount of HBO + 5mL distilled water test with litmus paper
2. Turmeric paper moistened with solution in no. 1

No visible change add a few crystals of HBO and dry

BO - brownish black
a. To the dry paper moisten with 15M NHOH. Observe the color change - greenish black
3. Evaporating dish - pinch amount of HBO + CHOH to dissolve + 1mL HSO mix
and set on fire
BO - HBO + 3CHOH (CH)BO + 3HO green bordered flame or green tint

INORGANIC PHARMACEUTICAL
MEDICINALS
C. Test for Impurities
1. Test for water insoluble substances : 1 g HBO + 10mL water
If clear - absence of water insoluble substance
2. Detect presence of
a. Na
- KHSbO
- Zn(UO)(CHCOO)
b. Cl
- AgNO

INORGANIC PHARMACEUTICAL
MEDICINALS
Preparation of Magnesium Carbonate, USP
LV

MgSO 7HO + NaCOHO (MgCO) Mg(OH) 5HO + Mg(HCO) +

NaSO + HO
Mg(HCO) +HO (MgCO) Mg(OH) 5HO + CO
HV
MgSO7HO + NaCOHO (MgCO)Mg(OH)5HO + NaSO + CO
+HO

INORGANIC PHARMACEUTICAL
MEDICINALS
A. Physical Properties
Describe the color, taste and relative bulk of the 2 varieties of the product
prepared
B. Test for Identity
1. Pinch amount + 5mL HCl - describe result
CO - (MgCO)Mg(OH)5HO + HCl MgCl + CO +HO effervescence

INORGANIC PHARMACEUTICAL
MEDICINALS
2. Sol'n in no. 1 + 1mL NHCl + 1mL NaHPO - describe the result
Mg
NHCl + NaHPO + MgCl MgNHPO + NaCl
(white crystalline)
Pinch amount of product + water + 2M NaOH (5 gtts) + titan
yellow (5 gtts) Mg(OH) red lake

INORGANIC PHARMACEUTICAL
MEDICINALS
3. Devise methods to identify the by product using the filtrate
in the preparation
a. Na
- KHSbO
- KHSbO
- Zn(UO)(CHCOO)
b. SO
- BaCl

INORGANIC PHARMACEUTICAL
MEDICINALS
Preparation of Potassium Iodide Saturated Solution
Physical Properties

Describe the odor, color, and taste

Reaction with litmus paper
Identity

3 gtts KISS + 10 gtts chloroform + 2gtts 3M sulfuric acid + KMnO4

Dilute 3gtts KISS with 3gtts water, acidify with 3gtts 6M CHCOOH + 3gtts NaNO shake
and 1gtt freshly prepared starch solution

5gtts HgCl + tin metal + excess KISS

INORGANIC PHARMACEUTICAL
MEDICINALS
Preparation of Potassium Acetate U.S.P.

CHCOOH + KHCO CHCOOK + CO + HO

A. Physical Properties
1. Form, color, odor & taste

INORGANIC PHARMACEUTICAL
MEDICINALS
B. Test for Identity
1. Aqueous soln. of KAc (0.5 in 10), divide into 2 portion
a. K
1st portion + NaCo(NO) dropwise until a change is observed
CHCOOK + NaCo(NO) KNaCo(NO) + NaCHCOO
(yellow cryst. ppt)
CHCOO
2nd portion + FeCl dropwise until distinct change is observed + acidify with 6M HCl
FeCl + CHCOOK Fe(CHCOO) + KCl acidify with HCl FeCl (red sol'n)
(yellow sol'n)

INORGANIC PHARMACEUTICAL
MEDICINALS
2. pinch amount CHCOOK + 5mL 3M HSO & heat - note odor
of vapors evolved
CHCOOK + HSO CHCOOH + KSO
(vinegar odor)
3. sol'n in (2) + 2mL 95% CHOH, heat in HO bath - note odor of
vapor evolved
CHCOOH + CHOH CHCOOCH + HO
(fruity odor)

INORGANIC PHARMACEUTICAL
MEDICINALS
4. Pyrolysis

Heating strongly an organic substance which decomposes into volatile

and inflammable vapors and leaves a residue containing particles of
carbon

Procedure:
Heat small amount of crystals in a crucible until change is observed
a. To the residue + 3M HSO dropwise - describe result

INORGANIC PHARMACEUTICAL
MEDICINALS
Pyrolysis
A. COMPLETE OXIDATION
CHCOOK + O KCO + CO + HO
(White residue)
KCO + HSO KSO + CO + HO
effervescence
B. INCOMPLETE OXIDATION
CHCOOK + O KCO + C + HO
(Black residue)
KCO + HSO KSO + CO + HO
effervescence

INORGANIC PHARMACEUTICAL
MEDICINALS

Preparation of Potassium Sodium Tartrate U.S.P

2KHCHO + NaCOHO +6HO 2KNaCHO4HO + CO
A. Physical Properties
Forms, color, odor & taste of the product

INORGANIC PHARMACEUTICAL
MEDICINALS
B. Test for Identity
1. 4mL mother liquor + 10mL HO, divided into 4 portions (1A, 1B, 2 & 3)
NO MOTHER LIQUOR
Product + 10mL HO divide into 4 portions (1A, 1B, 2 & 3)
a. 1st portion + 3-5gtts NaCo(NO) - describe result
K
2 KNaCHO4HO + NaCo(NO) KNaCo(NO) (s)

INORGANIC PHARMACEUTICAL
MEDICINALS
b. 2nd portion + 3-5 gtts KHSbO or KHSbO - describe result
Na
2KNaCHO4HO + KHSbO NaHSbO
(White ppt)
KNaCHO4HO + KHSbO NaHSbO
(White ppt)

INORGANIC PHARMACEUTICAL
MEDICINALS
2. 3rd portion + AgNO dropwise until ppt is formed + 6M NHOH
to dissolve ppt, heat in HO - observe results
CHO
KNaCHO +2AgNO AgCHO + KNO+ NaNO +4HO
(white ppt)
AgCHO + x'ss NHOH Ag(NH) heated Ag silver mirror
(colorless sol'n)

INORGANIC PHARMACEUTICAL
MEDICINALS
3. 4th portion + 6M CHCOOH dropwise until precipitation
CHO
KNaCHO4HO + CHCOOH KHCHO4HO + CHCOONa
White cryst ppt
Cream of Tartar

INORGANIC PHARMACEUTICAL
MEDICINALS

4. Pyrolysis

Small amount of crystals in crucible & heat until change is

observed
a. to the residue obtained + 3M HSO - observed result

INORGANIC PHARMACEUTICAL
MEDICINALS
A. COMPLETE OXIDATION
KNaCHO4HO +O KCO +NaCO + CO (g)+HO
(White residue)
KCO + HSO KSO + CO(g) + HO
(effervescence)
B. INCOMPLETE OXIDATION
KNaCHO4HO +O KCO +NaCO + CO(g) + C +HO
(Black residue)
KCO + HSO KSO + CO(g) + HO
effervescence

POST LABORATORY

ORAL REHYDRATION SALT

APPROXIMATE CONCENTRATION OF THE PRINCIPAL IONS IN THE PLASMA,
INTERSTITIAL AND INTRACELLULAR FLUIDS IN AN AVERAGE MAN

BODY
FLUIDS

Na

Ca

Mg

Cl

Plasma

140Mmol/L

4Mmol/L

2.5Mmol/L

1Mmol/L

102Mmol/L

27Mmol/L

1Mmol/L

Interstitial
Fluids

144

114

30

Intracellular
fluid

10

155

15

10

50

HCO HPO

CONCENTRATION & FUNCTION

OF GLUCOSE IN THE ORS
Glucose - absorbed through the intestinal wall
1 molecule glucose co transport 1 molecule of sodium
does not co-transport water
increased concentration of sodium across the intestinal wall
that pulls water through it
Sodium - carried by a co-transport mechanism

REASON WHY NOT ADVISABLE TO GIVE

COMMERCIAL DRINK (GATORADE) IN TREATING
DIARRHEA

Composition of ORS: Complex carbohydrates or 2% glucose 50 90 mmol/L sodium

Commercial drinks - do not meet these criteria and should not
be used for the purpose of treating diarrhea

ROLE OF POTASSIUM IN ORAL

REHYDRATION THERAPY
Repeated diarrhea - causes chronic loss of potassium resulting to
muscular weakness, lethargy & anorexia
Restoring potassium deficit - promotes a feeling of well being,
stimulates appetite & activity of the patient
Potassium unlike sodium - absorbed passively

REASON WHY BICARBONATE IS

INCLUDED IN THE ORS
Relevant for correction of metabolic acidosis of diarrheal
dehydration
Metabolic acidosis
Results whenever there is electrolyte imbalance & fluid loss
like in cases of diarrhea
Corrected by addition of potassium in the ORS

DOSE & DOSING REGIMEN OF

ORS
50mL/Kg Body
Weight

For mild dehydration every 4 hours

100mL/Kg Body
Weight

For moderate dehydration every 4 hours

10mL/kg Body
Weight

For diarrheal stool, after 4 hours, the patient is

reassessed

5mL

If patient is vomiting every 5 minutes

Increasing gradually as tolerated

PRECIPITATED SULFUR
Pale yellow, odorless, very fine amorphous powder with neutral reaction
to litmus
Solution is kept alkaline in the preparation precipitated sulfur
Flower of Sulfur
Contains small amount of AsS when digested with Ca(OH),
calcium arsenite & calcium sulfoarsenate [Ca(AsO) & Ca(AsS)]
2AsS + 6Ca(OH) Ca(AsO) + Ca(AsS) + 4HO + HS

PRECIPITATED SULFUR
if the solution is made acidic:
Ca(AsS) (calcium sulfoarsenate) - decomposes into insoluble AsS
which will again contaminate the precipitated sulfur
Ca(AsS) + 6HCl 3CaCl + AsS(s) + 3HS
Yellow ppt
Why is Precipitated Sulfur preferred over other kinds of Sulfur
Liquid mixture because the particles are lighter and more easily
suspended

OTHER FORMS OF SULFUR

Sublimed Sulfur or Flower of Sulfur or Azufre
Washed Sulfur
Allotropic Form
Rhombic
Monoclinic
Liquid or Mobile Sulfur
Plastic

USES OF SULFUR
Scabicide
Cathartic
Used in various skin disease for its keratolytic & fungicidal action
Dermatological agent in the treatment of:
Seborrhea (abnormal secretion of sebum from sebaceous gland giving an oily or
scaly appearance to the skin)
Acne
Psoriasis

BORIC ACID
Colorless, odorless, sour taste crystal/ powder/ scaly with a soapy feeling
Why is HCl used instead of HSO
HCl volatile acid, no residual traces will remain on the crystal surfaces
when dried
HSO non-volatile, less easily removed
Why is cold water used in washing the crystal?
Crystals are less soluble in cold water

USES

Eyewash or collyria
Bacteriostatic agent
Buffer component

BEFORE USE OF OFFICIAL SOLUTION

FOR OPHTHALMIC PURPOSE
Solution
Warmed or diluted with an equal volume of water, some will
crystallize out and should be dissolved otherwise it irritates
the eyes
Forms of Boric Acid preferred for preparing aqueous solution:
Crystalline/ Scaly Form - Soluble in water
Powder - tends to float on the surface of water

Calculate the volume of 12N HCl (D=1.185 d/mL

containing 36.31% by mass of HCl) necessary to react with
the amount of borax used in the preparation
NaBO10HO + 2HCl 4HBO + 2NaCl + 5HO
Theoretical mass of HCl from 30g NaBO10HO = 5.74g HCl
Vol of HCl: M = g/(MW x L)
L = 5.74g HCl / (12mol/L x 36.46g/mol)
= 13.1194 mL to react with borax
15mL of the HCl was used in the preparation:
15 - 13.1194 = 1.8806 excess vol of HCl used in the preparation

Calculate the volume of 12N HCl (D=1.185 g/mL

containing 36.31% by mass of HCl) necessary to react with
the amount of borax used in the preparation
12N HCl
Vol = wt/(sp. gr x % w/w)
= 5.74 g HCl /(1.185g/mL x 0.3631)
= 13.33 mL
15mL of the HCl was used in the preparation
15 - 13.33 = 1.67mL excess volume of HCl used in the preparation

MAGNESIUM CARBONATE
White amorphous powder, slightly carthly taste, bulky powder
Factors that determine the variety of MgCO prepared:
Amount of volume & temperature of the water used in the
preparation
Temperature at which the precipitate is dried

MAGNESIUM CARBONATE
Amount or volume and
temperature of the
water used in the
preparation

Temperature at which
the precipitate is
dried

LV

Cold water (62.5 mL)

Dried in a temp nmt

100C

HV

Boiling water (12.5 mL)

Dried without heat

Variety of
MgCO

USES:
Antacid
Laxative

POTASSIUM ACETATE
White crystalline powder, faint acetous odor, slightly alkaline taste
Amount of CHCOOH contained in 10mL of 6N CHCOOH
M = g/(MWxL)

g=M x MW x L

= 6mol/L x 36g/mol x 0.01L = 3.6g HAc

Grams of KHCO needed to react with CHCOOH in the experiment
CHCOOH + KHCOCHCOOK + CO + HO
=

3.6 g HAc
1mol HAc / 60g HAc
= 6 g KHCO

1 mol KHCO
1 mol HAc

100.11 g KHCO
1 mol KHCO

POTASSIUM ACETATE
Purpose of Sandbath
To increase the temperature to over 100C and to exceed 140C
during the evaporation of CHCOOK
Reason why CHCOOK is bottled immediately
Deliquescent in nature
Therapeutic Uses
Diuretic and Antacid

ROCHELLE SALT/ SEIGNETTE SALT/

POTASSIUM SODIUM TARTRATE
White crystalline powder or colorless rhombic prism with saline cooling
taste
Implications if in the pyrolysis of the crystals there are Carbon remaining
There is no ample supply of oxygen or if heating is insufficient some
black carbon particles that will remain
Medicinal Use:
Components of Seidlitz powder which is used as a cathartic,
Mild laxative
Potent hydraqogue (depending on the dose administered)

ROCHELLE SALT/ SEIGNETTE SALT/

POTASSIUM SODIUM TARTRATE
Fehling's Solution
Alkaline CuCHO
Example of chelate complexation where the concentration Cu is
very little and is not precipitated by NaOH present in the reagent
Property of the tartrate ion is utilized in Fehling's solution
Sequestration or chelate complexation
Tartrate chelate Cu