Quality Control Of N Acetylcysteine Biology Essay

N-acetylcysteine ( C5H9NO3S Mr 163.2 ) is the N-acetyl derived function of the of course happening amino acid, l-cysteine. The drug occurs as a white, crystalline pulverization with a little acetic olfactory property. N-acetylcysteine is freely soluble in H2O and in intoxicant. N-acetylcysteine is commercially available as aqueous solutions of the Na salt of the drug. It is used as a mucolytic or as an counterpoison for paracetamol. The British Pharmacopoeia contains a figure of trials for this compound designed to guarantee the quality.

N-acetylcysteine Acts of the Apostless to cut down mucous secretion viscousness by dividing disulfide bonds associating proteins present in the mucous secretion ( mucoproteins ) . Inhaled N-acetylcysteine is indicated for mucolytic ( “ mucus-dissolving ” ) therapy as an adjuvant in respiratory conditions with inordinate and/or thick mucous secretion production. Such conditions include emphysema, bronchitis, TB, bronchiectasis, amyloidosis, pneumonia. It is besides used post-operatively, as a diagnostic assistance, and in tracheostomy attention. It may be considered uneffective in cystic fibrosis ( Rossi, 2006 ) . However, a recent paper in the Proceedings of the National Academy of Sciences studies that high-dose unwritten N-acetylcysteine modulates redness in cystic fibrosis and has the possible to counter the intertwined oxidation-reduction and inflammatory instabilities in CF ( Tirouvanziam et al. , 2006 ) . Oral N-acetylcysteine may besides be used as a mucolytic in less serious instances.

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N-acetylcysteine besides acts to augment glutathione militias ( depleted by toxic paracetamol metabolites ) in the organic structure and, together with glutathione to straight adhere to toxic metabolites. These actions serve to protect hepatocytes in the liver from toxicity due to paracetamol overdose. Intravenous N-acetylcysteine is indicated for the intervention of paracetamol ( Datril ) overdose. Oral N-acetylcysteine for this indicant is uncommon as it is ill tolerated owing to the high doses required ( due to hapless unwritten bioavailability ) , unpleasant gustatory sensation or smell and inauspicious drug reactions ( peculiarly sickness and emesis ) . However, some people have shown an inauspicious allergic reaction to endovenous N-acetylcysteine which includes utmost take a breathing trouble, light-headedness, roseolas, terrible coughing and sometimes besides purging. Repeated overdoses will do the allergic reaction to acquire worse and worse.

N-acetylcysteine is prone to both hydrolysis and oxidization and some of the drosss from these reactions are shown below.

Scheme 2

2. Experimental:

2.1. Materials:

2.1. Materials:

The stuffs used in this experiment were N-acetylcysteine pulverization, disodium edentate solution, 1M Na hydrated oxide and assorted phosphate buffer pH 7.0, H2O, dilute hydrochloric acid, K iodine solution, 0.05M I, 0.1M Na hydrated oxide, amylum, phenol ruddy and phenolphthalein as indexs.

The setup used were optical rotary motion analyzer, conelike flasks, 10mL and 50mL pipettes, burette, electronic weigh balance and beakers.

2.2. Methods:

a ) Specific optical rotary motion: +21IS to +27IS

1.25g N-acetylcysteine pulverization was weighed and allowed dissolve in a mixture of 1ml of 10g/L solution of disodium edentate, 7.5ml of 1M Na hydrated oxide and sufficient sum of assorted phosphate buffer pH 7.0 to 25ml entire volume. Optical rotary motions of the freshly prepared solution and the old solutions of N-acetylcysteine provided were measured and recorded.

B ) Assay: 98.0 % -101.0 % C5H9NO3S ( as dried stuff )

0.14g N-acetylcysteine pulverization was weighed by difference and poured into a conelike flask. 60 milliliter of H2O and 10ml dilute hydrochloride acid were measured and added into the conelike flask. The conelike flask was agitating to guarantee the N-acetylcysteine pulverization was to the full dissolved. The solution was left to chill. Another 10ml of K iodide solution was added into the cooled solution in the conelike flask. The solution was so titrated with 0.05M I by utilizing amylum as index. Second titration was carried out to guarantee accurate and precise consequence.

degree Celsius ) Assay by titration with 0.1M Na hydrated oxide

0.3g N-acetylcysteine pulverization was weighed by difference and poured into a clean conelike flask. Approximately 50 milliliter of distilled H2O was measured and added into the conelike flask. The conelike flask was agitating to guarantee the N-acetylcysteine pulverization was to the full dissolved. The solution was titrated with 0.1M Na hydrated oxide utilizing phenol ruddy as index. Second titration was carried out to guarantee accurate and precise consequence.

0.3g N-acetylcysteine pulverization was weighed by difference and poured into a clean conelike flask. Approximately 50 milliliter of distilled H2O was measured and added into the conelike flask. The conelike flask was agitating to guarantee the N-acetylcysteine pulverization was to the full dissolved. The solution was titrated with 0.1M Na hydrated oxide utilizing phenolphthalein as index. Second titration was carried out to guarantee accurate and precise consequence.

vitamin D ) Zinc: Not more than 10ppm Zincs

1.00g of N-acetylcysteine pulverization was weighed and dissolved in 0.001M hydrochloric acid. The solution was diluted to 50ml with 0.001M hydrochloric acid and solution 1 was obtained.

Three solutions were prepared for analysis. The first solution consists of 10ml solution 1 diluted to 20ml with 0.001M hydrochloric acid, 2nd solution consists of 10ml solution 1 and 1ml of 5ppm zinc criterion diluted to 20ml with 0.001M hydrochloric acid and the 3rd solution consists of 10ml solution 1 and 2ml of 5ppm zinc criterion diluted to 20ml with 0.001M hydrochloric acid.

The optical density of each solution was measured at 213.8nm utilizing an atomic soaking up spectrophotometer. The optical density for each solution was tabulated. The Zn content in each sample was calculated utilizing the method of standard add-on.

vitamin E ) Loss on drying: Not more than 1.0 % w/w

A sample of N-acetylcysteine was dried at 70IS C in vacuo for 3 hours and the information was recorded and the per centum loss on drying of this sample was calculated.

degree Fahrenheits ) Related substances

The chromatograms obtained from the HPLC analysis of both fresh solution and old solution of N-acetylcysteine was examined.

3. Consequences:

a ) Specific optical rotary motion:

Mass of weighing boat ( g )

26.6089

Mass of weighing boat + sample ( g )

27.8609

Mass of weighing boat + residue ( g )

26.6079

Mass of sample transferred ( g )

1.253

Table 1: The mass of N-acetylcysteine used to do a solution for measuring of specific optical rotary motion.

Calculations:

Harmonizing to British Pharmacopoeia ( BP 1999 ; page 40-41 ) , it states that the specific optical rotary motion is +A 21.0 to +A 27.0. To obtain the angle of rotary motion, the equation below is used,

Where, [ I± ] = specific optical rotary motion

I± = observed angle of rotary motion

C = concentration of active substance in g/100mL of the solution

cubic decimeter = length of column in 2dcms

For newly prepared solution:

Angle obtained ( I± ) : 2.45a?°

Concentration of N-acetylcysteine ( degree Celsius ) : 5.012 % w/v

Path length = 2 diabetes mellitus

Specific optical rotary motion:

= 100 tens 2.45a?°

2 x 5.012g/ml

= +24.5a?°

For old solution:

Angle obtained ( I± ) : -3.29a?°

Concentration of N-acetylcysteine ( degree Celsius ) : 5.012 % w/v

Path length = 2 diabetes mellitus

Specific optical rotary motion:

= 100 tens 3.29a?°

2 x 5.012g/ml

= -32.9a?°

B ) Assay: 98.0 % -101.0 % C5H9NO3S ( as dried stuff )

Sample 1

Sample 2

Mass of boat + sample ( g )

3.8797

3.8777

Mass of boat + residue ( g )

3.7393

3.7398

Mass of Acetylcysteine transferred ( g )

0.1404

0.1379

Table 2: The mass of N-acetylcysteine pulverization in sample 1 and sample 2 for titrations with I.

First reading

Second reading

Initial volume ( milliliter )

17.40

26.70

Concluding volume ( milliliter )

26.40

35.50

Volume of 0.05M I used ( milliliter )

9.00

8.80

Table 3: The volume of I used for both titration utilizing sample 1 and sample 2 of N-acetylcysteine solution and amylum as index.

Calculations:

Actual concentration of I used: 0.0476M

Molecular weight of N-acetylcysteine ( C5H9NO3S ) : 163.2

The balanced equation for the reaction between N-acetylcysteine and I:

2 C5H9NO3S + I2 a C5H8NO3SSC5H8NO3 + 2HI

2KI a I2 + 2K+

Harmonizing to British Pharmacopoeia, 1mL of 0.05M I is tantamount to 16.32mg of C5H9NO3S. This means, 2 mole of C5H9NO3S equal to one mole of I.

Therefore when 1mL of 0.05M iodine = 16.32mg of C5H9NO3S,

1mL of 0.0476M iodine = 0.0476M ten 16.32mg/ 0.05M

= 15.54mg of C5H9NO3S

First titration:

1mL of 0.0476M iodine = 15.54mg of C5H9NO3S

So, 9.00mL of 0.0476M iodine = 9.00mL ten 15.54mg/ 1mL

= 139.86mg

= 0.13986g of C5H9NO3S

Second titration:

1mL of 0.0476M iodine = 15.54mg of C5H9NO3S

So, 8.80mL of 0.0476M iodine = 8.80mL ten 15.54mg/ 1mL

= 135.52mg

= 0.13552g of C5H9NO3S

Calculation of Percentage of Purity:

Sample 1 of N-acetylcysteine

Sample 2 of N-acetylcysteine

Mass transferred

Actual mass calculated

Mass transferred

Actual mass calculated

0.1404

0.1399

0.1379

0.1355

Harmonizing to British Pharmacopoeia ( BP ) , the per centum of pureness should be within 98.0 – 101.0 % of dried substance.

Equation of the Percentage of Purity:

Sample 1:

Sample 2:

degree Celsius ) Assay by titration with 0.1M of Na hydrated oxide

I ) Titration by utilizing phenol ruddy index

Sample 1

Sample 2

Mass of boat + sample ( g )

3.8916

3.9199

Mass of boat + residue ( g )

3.5913

3.6198

Mass of N-acetylcysteine transferred ( g )

0.3003

0.3001

Table 4: The mass of N-acetylcysteine pulverization in sample 1 and sample 2 for titrations with 0.1M of Na hydrated oxide.

First reading

Second reading

Initial volume ( milliliter )

1.00

1.00

Concluding volume ( milliliter )

18.15

18.10

Volume of 0.05M I used ( milliliter )

17.15

17.10

Table 5: The volume of 0.1M Na hydrated oxide used for both titration utilizing sample 1 and sample 2 of N-acetylcysteine solution and phenol ruddy as index.

Calculations:

Actual concentration of Na hydrated oxide ( NaOH ) used: 0.1062M

Molecular weight of N-acetylcysteine ( C5H9NO3S ) : 163.2

The balanced equation for the reaction between N-acetylcysteine and Na hydrated oxide ( NaOH ) :

C5H9NO3S + NaOH a C5H8NO3SNa + H2O

From the equation, one mole of N-acetylcysteine reacts with one mole of NaOH. So the reaction is a 1:1 ratio. To happen out the figure of mole of NaOH, the equation below is used:

First titration:

Gram molecules of NaOH = ( 0.1062M x 17.15mL ) /1000

= 1.821 x10-3 moles

As the reaction is 1:1 ratio so the figure of moles of N-acetylcysteine is equal to the figure of moles of NaOH used which is 1.821 x10-3 mole.

Mass of N-acetylcysteine = 1.821 x10-3 moles x 163.2

= 0.2972g

Second titration:

Gram molecules of NaOH = ( 0.1062M x 17.10mL ) /1000

= 1.816 x10-3 moles

As the reaction is 1:1 ratio so the figure of moles of N-acetylcysteine is equal to the figure of moles of NaOH used which is 1.821 x10-3 mole.

Mass of Acetylcysteine = 1.816 x10-3 mole ten 163.2

= 0.2964g

Calculation of Percentage of Purity:

Sample 1 of N-acetylcysteine

Sample 2 of N-acetylcysteine

Mass transferred

Actual mass calculated

Mass transferred

Actual mass calculated

0.3003

0.2972

0.3001

0.2964

Harmonizing to British Pharmacopoeia ( BP ) , the per centum of pureness should be within 98.0 – 101.0 % of dried substance.

Equation of the Percentage of Purity:

Sample 1:

Sample 2:

two ) Titration by utilizing Phenolphthalein as the index

Sample 1

Sample 2

Mass of boat + sample ( g )

3.8916

3.9195

Mass of boat + residue ( g )

3.5915

3.6195

Mass of N-acetylcysteine transferred ( g )

0.3001

0.3000

Table 6: The mass of N-acetylcysteine pulverization in sample 1 and sample 2 for titrations with 0.1M of Na hydrated oxide.

First reading

Second reading

Initial volume ( milliliter )

18.20

17.10

Concluding volume ( milliliter )

36.80

36.95

Volume of 0.05M I used ( milliliter )

18.60

19.85

Table 7: The volume of 0.1M Na hydrated oxide used for both titration utilizing sample 1 and sample 2 of N-acetylcysteine solution and phenolphthalein as index.

Calculations:

Actual concentration of Na hydrated oxide ( NaOH ) used: 0.1062M

Molecular weight of N-acetylcysteine ( C5H9NO3S ) : 163.2

The balanced equation for the reaction between N-acetylcysteine and Na hydrated oxide ( NaOH ) :

C5H9NO3S + NaOH a C5H8NO3SNa + H2O

From the equation, one mole of a N-acetylcysteine reacts with one mole of NaOH. So the reaction is a 1:1 ratio. To happen out the figure of mole of NaOH, the equation below is used:

First titration:

Gram molecules of NaOH = ( 0.1062M x 18.60mL ) /1000

= 1.975 x10-3 mole

As the reaction is 1:1 ratio so the figure of moles of N-acetylcysteine is equal to the figure of moles of NaOH used which is 1.821 x10-3 mole.

Mass of N-acetylcysteine = 1.975 x10-3 mole ten 163.2

= 0.3224g

Second titration:

Gram molecules of NaOH = ( 0.1062M x 19.85mL ) /1000

= 2.108 x10-3 mole

As the reaction is 1:1 ratio so the figure of moles of N-acetylcysteine is equal to the figure of moles of NaOH used which is 1.821 x10-3 mole.

Mass of N-acetylcysteine = 1.816 x10-3 mole ten 163.2

= 0.3440g

Calculation of Percentage of Purity:

Sample 1 of N-acetylcysteine

Sample 2 of N-acetylcysteine

Mass transferred

Actual mass calculated

Mass transferred

Actual mass calculated

0.3001

0.3224

0.3000

0.3440

Calculation of Percentage of Purity:

Harmonizing to British Pharmacopoeia ( BP ) , the per centum of pureness should be within 98.0 – 101.0 % of dried substance.

Equation of the Percentage of Purity:

Sample 1:

Sample 2:

vitamin D ) Zinc: Not more than 10ppm Zinc ( Zn ) :

To find the concentration of Zinc metal nowadays in a standardized sample, atomic soaking up spectrophotometer was applied. This was done so as to follow with the British Pharmacopoeia ( BP ) criterions, where the detected concentration of Zinc should non be more than 10ppm.

Mass of Acetylcysteine sample used: 1.00g

This sample was diluted consequently and so analysed or measured by an atomic soaking up spectrophotometer at a set wavelength of 213.8nm. Harmonizing to the research lab transcript, the optical densities were given, so the computation was carried out to find the concentrations for each solution.

Solution

Concentration ( mg/L )

Optical density ( at 213.8nm )

( a )

0.00

0.056

( B )

0.25

0.115

( degree Celsius )

0.50

0.173

Table 8: The optical density of solution a, B and degree Celsius utilizing atomic optical density spectrophotometer.

From the tabular array 8 above, a standard add-ons standardization graph of concentration of Zn in mg/L against optical density at 213.8nm is plotted. A instead little optical density indicates that there is a hint or little sum of Zinc ( Zn ) nowadays in Solution A, which practically contained merely the N-acetylcysteine sample. Hence, we can plot a line of best tantrum and extrapolate to happen the concentration of Zn nowadays within our sample. Note that the sum of Zn nowadays is relative to the optical density detected at 213.8nm wavelength.

Graph 1: The graph of optical density against concentration of Zinc.

Extrapolated value= -0.24 Solution A = 0.24ppm Solution 1 = 0.24 A- 2 = 0.48 ppm

Solution 1

0.48g in 100 000 milliliter = 2.4 A- 10-4g in 50 milliliter

If 1g of N-acetylcysteine contains 2.4 A- 10-4g of Zn ions, 104g of acetylcysteine will incorporate 2.4g of Zn ions.

So concentration of Zn ions in N-acetylcysteine = 2.4ppm

Using the standardization graph, we obtained an equation for the line of best tantrum as shown below:

Using the line of best tantrum we can cipher the concentration of Zinc ( Zn ) nowadays within Solution 1. This is determined by the difference between the beginning ( ten = 0 ) and where the line of best tantrum intercepts the x-axis. To be more accurate, the equation of the line of best tantrum can be used by presuming the optical density of N-acetylcysteine at 213.8nm ( y-axis ) is 0 ( Y = 0 ) . We can so cipher and happen the exact concentration of Zn added ( x-axis in mg/L ) which gives an optical density reading of 0.0562 at the wavelength of 213.8 nanometer. This computation is shown below where optical density Y = 0.

Concentration of Zinc in solution ( a ) where no Zinc is added: –

( Concentration comes in positive value )

Therefore, the diluted Solution 1 contains an exact concentration of 0.2402mgL-1 or 0.2402ppm. We can now utilize this concentration and work backwards from the dilution to obtain the mass of Zn within the 20mL Solution 1, as shown in the computation below,

Mass of Zinc in Solution 1: –

From the mass of Zinc nowadays in Solution 1 as calculated, we can state that this peers to the 10mL of N-acetylcysteine sample in Solution ( a ) . This is because Solution 1 was diluted to 20mL utilizing 0.001M hydrochloric acid and contained no other beginnings of Zinc. Hence, 4.8034I?g of Zinc in 20mL of Solution 1 is equal to 4.8034I?g of Zinc in 10mL of Solution ( a ) . Now utilizing this mass of 4.8034I?g in 10mL of Solution ( a ) we can happen out the entire mass of Zinc within 50mL. However, the entire mass of Zinc within 50mL of Solution ( a ) is tantamount to 1.00g of N-acetylcysteine sample which is the original sample mix. Using these informations, the mass of Zinc can be calculated as shown in the computation below,

Mass of Zinc in 1.00g of N-acetylcysteine: –

Hence, 2.4017I?gmL-1 of Zinc is present in 1.00g. We can now cipher an exact concentration of Zinc in parts per million ( ppm ) as shown in the computation below,

Concentration of Zinc within sample in ppm: –

vitamin E ) Loss on drying: Not more than 1.0 % w/w: –

Initial mass of N-acetylcysteine sample ( g )

1.0965

Mass after drying under specified conditions ( g )

1.0893

degree Fahrenheits ) Related substances

1 ) Acetylcysteine: fresh sample 8.57mg/mL

From British Pharmacopoeia, the keeping clip for the N-acetylcysteine substances as below.

Substance

Retention clip ( min )

L- cystine

About 2.2

L- cysteine

About 2.4

2-methyl-2 thiazoline-4 carboxylic acid

About 3.3

N, N’-diacetyl-L- cystine

About 12

N, N’-diacetyl-L- cysteine

About 14

acetylcysteine

About 6.4

1 ) Acetylcysteine: fresh sample 8.57mg/mL

Substance

Retention clip ( min )

Peak keeping clip obtained

Concentration

L- cystine

About 2.2

1.93

0.5948

L- cysteine

About 2.4

2-methyl-2 thiazoline-4 carboxylic acid

About 3.3

3.25

0.0794

N, N’-diacetyl-L- cystine

About 12

N, N’-diacetyl-L- cysteine

About 14

13.623

0.3944

Acetylcysteine

About 6.4

6.972

94.7507

Calculation of drosss:

Peak area/ Total country x 100

Substance

Area

Concentration

Impurity

L- cystine

238606

0.5948

0.5948

L- cysteine

2-methyl-2 thiazoline-4 carboxylic acid

31861

0.0794

0.0794

N, N’-diacetyl-L- cystine

N, N’-diacetyl-L- cysteine

158211

0.3944

0.3944

Acetylcysteine

38007440

94.7507

94.7507

Entire area= 40113072

2 ) Acetylcysteine: old sample 2.5mg/mL

Substance

Retention clip ( min )

Peak keeping clip obtained

Concentration

L- cystine

About 2.2

2.11

0.7214

L- cysteine

About 2.4

2-methyl-2 thiazoline-4 carboxylic acid

About 3.3

3.256

0.8946

N, N’-diacetyl-L- cystine

About 12

N, N’-diacetyl-L- cysteine

About 14

13.415

15.3284

Acetylcysteine

About 6.4

6.34

33.7241

Calculation of drosss:

Peak area/ Total country x 100

Substance

Area

Concentration

Impurity

L- cystine

62935

0.7214

0.7214

L- cysteine

2-methyl-2 thiazoline-4 carboxylic acid

78046

0.8946

0.8946

N, N’-diacetyl-L- cystine

N, N’-diacetyl-L- cysteine

1337263

15.3284

15.3284

Acetylcysteine

2942118

33.7241

33.7241

Entire area= 8724087

3 ) Cysteine/ cystine: 0.5mg/mL

Substance

Retention clip ( min )

Peak keeping clip obtained

Concentration

L- cystine

About 2.2

2.018

5.2956

L- cysteine

About 2.4

2.323 ; 2.65

2.3189 ; 2.384

2-methyl-2 thiazoline-4 carboxylic acid

About 3.3

3.008 ; 3.207

24.9029 ; 65.0987

N, N’-diacetyl-L- cystine

About 12

N, N’-diacetyl-L- cysteine

About 14

Acetylcysteine

About 6.4

Calculation of drosss:

Peak area/ Total country x 100

Substance

Area

Concentration

Impurity

L- cystine

87001

5.2956

5.2956

L- cysteine

38097 ; 39167

2.3189 ; 2.384

2.3189 ; 2.384

2-methyl-2 thiazoline-4 carboxylic acid

409128 ; 1069503

24.9029 ; 65.0987

24.9029 ; 65.0987

N, N’-diacetyl-L- cystine

N, N’-diacetyl-L- cysteine

Acetylcysteine

Entire area= 1642895

4. Discussion:

a ) Specific optical rotary motion:

The specific rotary motion of a chemical compound [ I± ] is defined as the ascertained angle of optical rotary motion I± in stereochemistry, when plane-polarized visible radiation is passed through a sample with a way length of 1 decimeter ( diabetes mellitus ) and a sample concentration of 1 gm ( g ) per 1 milliliter ( milliliter ) . The specific rotary motion of a pure stuff is an intrinsic belongings of that stuff at a given wavelength and temperature. The reading should be accompanied by the temperature at which the measuring was performed and the dissolver in which the stuff was dissolved, and this frequently assumed to be room temperature. The exact unit for specific rotary motion values is deg dma?’1cm3 ga?’1 or can utilize grades ( IS ) . Levorotary rotary motion ( cubic decimeter ) means a negative reading obtained and the rotary motion being to be left. While dextrorotary rotary motion ( vitamin D ) means a positive reading and the rotary motion is being to be right. The specific optical rotary motion for the newly prepared solution of N-acetylcysteine is +24.5a?° which it is dextrorotary rotary motion and the old solution of N-acetylcysteine is -32.9a?° which means levorotary rotary motion.

Measurement of optical rotary motion is a manner to measure optical pureness of a sample incorporating a mixture of enantiomorphs. An enantiomorph is one of two stereoisomers that are mirror images of each other that are “ non-superposable ” or non indistinguishable much as one ‘s left and right custodies are “ the same ” but face-to-face. The specific optical rotary motion of N-acetylcysteine solution is within the scope +21IS to about +27IS . The newly prepared of N-acetylcysteine solution is found to be in the scope nevertheless the old N-acetylcysteine solution is non in the scope. This reveals stableness change occurred in the old N-acetylcysteine solution. The drosss have found in the old N-acetylcysteine solution because the presence of little sum of drosss can impact the rotary motion of the sample.

The existent optical rotary motion value for newly prepared N-acetylcysteine solution is measured by individual polariscope because if the sample is really concentrated or it has really big specific rotary motion or the sample larger than 180A° , individual polariscope can non be used. The fluctuation of specific rotary motion with wavelength is the footing of optical rotary scattering ( ORD ) which used to clarify the absolute constellation of certain samples. High public presentation liquid chromatography ( HPLC ) is used to find the enantiomeric ratio with a chiral column because the collection in the N-acetylcysteine solution cause optical rotary motion of a sample possibly non additive dependant due to enantiomeric surplus.

B ) Assay: 98.0 % -101.0 % C5H9NO3S ( as dried stuff )

From the consequence obtained above, the mass obtained from the titration of N-acetylcysteine solution with I with amylum as index for first titration is 0.13986g and 2nd titration is 0.13552g. The per centum of pureness obtained from the experiment for first sample is 99.64 % . The per centum of pureness from 2nd sample is 98.26 % . Harmonizing to British Pharmacopoeia ( BP ) , the per centum of should be within 98.0 – 101.0 % of dried substance. The per centum of pureness for both samples is within the scope stated in the BP. BP prefer the iodine titration to a titration utilizing Na hydrated oxide because I is a really utile oxidizing titrant which react with cut downing agent, N-acetylcysteine solution utilizing amylum as index. Iodine forms an intensely dark blue composite with amylum. Starch is an oxidization – decrease index that shows a reversible coloring material alteration between the oxidized and decreased signifiers. It is non affected by the presence of iodide ( I- ) . Both amylum and iodide must be present for the amylum to alter coloring material during the titration. Iodine is consumed by thiosulfate in the titration measure. The sum of thiosulfate used is relative to the sum of I liberated from the salt. Sodium hydrated oxide is a strong base. It is more utile in acid- base titration utilizing weak acid or base index.

degree Celsius ) Assay by titration with 0.1M of Na hydrated oxide

From the consequence obtained in this experiment, the mass obtained from the titration of N-acetylcysteine solution with0.1M Na hydrated oxide with phenol ruddy as index for first titration is 0.2972g and 2nd titration is 0.2964g. The per centum of pureness obtained from the experiment for first sample is 98.97 % . The per centum of pureness from 2nd sample is 98.77 % . Harmonizing to British Pharmacopoeia ( BP ) , the per centum of should be within 98.0 – 101.0 % of dried substance. The per centum of pureness for both samples is within the scope stated in the BP.

The mass obtained from the titration of N-acetylcysteine solution with 0.1M Na hydrated oxide with phenolphthalein as index for first titration is 0.3224g and 2nd titration is 0.3440g. The per centum of pureness obtained from the experiment for first sample is 107.43 % . The per centum of pureness from 2nd sample is 114.67 % . Harmonizing to British Pharmacopoeia ( BP ) , the per centum of should be within 98.0 – 101.0 % of dried substance. The per centum of pureness for both samples is out of the scope stated in the BP.

Phenol ruddy and phenolphthalein are acid-base indexs. The un-dissociated signifier of the index is a different coloring material than the iogenic signifier of the index. An Index does non alter coloring material from pure acid to pure alkaline at specific H ion concentration, but instead, color alteration occurs over a scope of H ion concentrations. This scope is termed the coloring material alteration interval. It is expressed as a pH scope. The pH scope for phenol ruddy is 6.8- 8.4 and phenolphthalein is 8.0- 10.0. The choice of index will depend on the existent expected pH at the equality point which selects an index with a pKa right in the center of the pH alteration at the equality point. N-acetylcysteine solution has pKa 4.0 and 9.5, and a weak acid index has to be used to find the terminal point of the titration. Phenol ruddy green goods a good consequence compared to the phenolphthalein as index when titrate N-acetylcysteine solution with 0.1M Na hydrated oxide.

vitamin D ) Zinc: Not more than 10ppm Zinc ( Zn ) :

By executing the atomic optical density technique, we have determined that the N-acetylcysteine sample contained a Zinc concentration of 2.4017ppm. This sample complied with the demand from the British Pharmacopoeia ( BP ) monograph criterions by non holding a Zinc concentration of greater than 10ppm.

Atomic optical density technique can merely observe specifically one heavy metal at a clip. So, it is really clip devouring to observe a broad spectrum of heavy metal drosss within our sample. Plus, the N-acetylcysteine monograph merely indicates the demand to supervise the degree of Zinc nowadays within the sample by atomic optical density spectroscopy. Therefore, to observe other heavy metals we would prefer to utilize the more generic “ Limit Test C for Heavy Metallic elements ” as specified in the British Pharmacopoeia ( 2008 ) , Volume IV, and Appendix VII.

vitamin E ) Loss on drying: Not more than 1.0 % w/w: –

Harmonizing to British Pharmacopoeia ( BP ) , it states that there should be no more than 1.0 % in mass. This sample is complied with the BP monograph criterions with a loss of merely 0.66 % in mass.

degree Fahrenheits ) Related substances: –

HPLC is used in pharmaceutical analysis to quantitative findings of drugs in preparations. These analyses do non necessitate long clip to optimizing nomadic stage and choosing columns and sensors. Some preparations contain more than one active ingredient and may show more of an analytical challenge since the different ingredients may hold rather different chemical belongingss and elute at really different times from HPLC column.

5. Decisions:

Quality control is an indispensable operation of the pharmaceutical industry. Drugs must be marketed as safe and therapeutically active preparations whose public presentation is consistent and predictable. A package of sophisticated analytical methods are being developed for the drugs rating in pharmaceutical industry. Requirements regulating the quality control of pharmaceuticals in conformity with the British Pharmacopoeia ( BP ) or European Pharmacopoeia.

Titration is a process used in chemical science in order to find the molar concentration of an acid or a base. A chemical reaction is set up between a known volume of a solution of unknown concentration and a known volume of a solution with a known concentration. The comparative sourness ( basicity ) of an aqueous solution can be determined utilizing the comparative acid ( base ) equivalents. For a decently performed titration, the volume difference between the terminal point and the equality point is little. Sometimes the volume difference ( mistake ) is ignored ; in other instances a rectification factor may be applied.

High public presentation liquid chromatography ( HPLC ) is the technique most normally used for the quantitation of drugs in preparations. Pharmacopoeial checks still rely on direct UV spectrometry but in industries, sensing by UV spectrophotometry is normally combined with a preliminary separation by HPLC. The combination of high force per unit area liquid chromatography with monitoring by UV or seeable sensing provides an accurate, precise and robust method for quantitative analysis of pharmaceutical merchandises.