Levofloxacin Hemihydrate

PURPOSE:-

To describe Raw material testing procedure of Levofloxacin Hemihydrate.

SCOPE:-

This procedure pertains to testing of Levofloxacin Hemihydrate.

Molecular Weight:-

370.38 g/mol

Chemical Structure:-

Levofloxacin Hemihydrate
Levofloxacin Hemihydrate

IUPAC NAME:-

(3S)-9-Fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid hemihydrate

RESPONSIBILITY:-

It is the responsibility of Analyst to follow this procedure while performing testing.

It is responsibility of Supervisor to make certain that this procedure is followed in its entirety.

It is responsibility of Manager to review and make changes where applicable.

EQUIPMENTS / INSTRUMENTS:-

HPLC

FTIR

Muffle Furnace

L.O.D Apparatus

MATERIALS / CHEMICALS:-

Dimethyl sulfoxide

Acetic Acid

Distilled Water

Acetone

Methanol

Glycerin

Octanol

Cupric Sulfate Pentahydrate

L-Ammonium Acetate

L-Isoleucine in Water

Methanol 

DESCRIPTION (USP)

Light yellowish white to yellow white crystals or powder.

CONTENTS:-

Contents are 98.0% to 102.0 %

SOLUBILITY (USP)

Sparingly soluble in water, acetone and methanol.

Soluble in Dimethyl sulfoxide and acetic acid.

Practically insoluble in Glycerin and octanol.

IDENTIFICATION BY FTIR SPECTROPHOTOMETER:-

Measure the FTIR spectra of sample and compare with standard.

The Retention time of the major peak of the sample solution corresponds to the standard solution as obtained in the assay.

QUANTITATIVE ASSAY

PROCEDURE:-

Preparation Of Buffer:-

8.5 mg/Litr ammonium acetate

1.25 grm/ Litr of Cupric Sulfate Pentahydrate

1.3 grm/Litr of L-Isoleucine in water

Preparation Of Mobile Phase:

Methanol and Buffer ( 3:7 )

Preparation Of Standard Solution:

Weigh 50mg of the Levofloxacin Hemihydrate RS and transfer it into 50ml of volumetric flask. Add mobile phase in it and sonicate to dissolve. Then make the volume up to the mark. Then filter the solution.

Preparation Of Sample Solution:-

Weigh 50mg of the Levofloxacin Hemihydrate (Raw Material) and transfer it into 50ml of volumetric flask.  Add mobile phase in it and sonicate to dissolve. Then make the volume up to the mark. Then filter the solution.

Chromatographic Conditions

Column        :           4.6mm x 25cm x Packing L1

Detector       :           UV at 360nm

Column Temperature :        45°C

Flow Rate    :           0.8ml/Min

Injection Size:          25µL

CALCULATIONS:-

Calculate the Percentage of  Levofloxacin Hemihydrate by using following Expression.

Where

ru = Peak Response from the sample solution

rs =  Peak Response from the standard solution

Cs = Concentration of Levofloxacin Hemihydrate in th standard solution (mg/ml)

Cu =   Concentration of Levofloxacin Hemihydrate in th sample solution (mg/ml)

P= Potency of Standard

 

L.O.D:-

2.0%  – 3.0% 

OPTICAL ROTATION:-

Solvent methanol

50mg/ml in solvent.

92° – 106° at 20°C

REFERENCE DOCUMENTS

United State Pharmacopeia, USP 41,NF 36, Volume III, Page No.2395-7. for Levofloxacin

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  1.  Amoxicilline Hydrate                 2.  Vitamin-C

 

Amoxicillin Hydrate

Amoxicillin

is a semisynthetic aminopenicillin antibiotic with bactericidal activity. It is used as Amixicillin Hydrate Amoxicillin binds to and inactivates penicillin-binding protein (PBP) 1A located on the inner membrane of the bacterial cell wall.

IUPAC  Name

IUPAC name of Amoxicillin Hydrate is

(2S,5R,6R)-6-[[(2R)-2-amino-2-(4-hydroxyphenyl)acetyl]amino]-3,3-dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid, trihydrate 

Molecular Formula

C16H19N3O5S • 3H2O

Chemical Structure

Amoxicillin
Amoxicillin Hydrate

Formula Weight

419.4 

Purity

≥98%

Physical Appearance:

Amoxicillin Hydrate occurs as white to light yellowish white, crystals or crystalline powder.

Solubility

It is slightly soluble in water and in methanol, and very slightly soluble in ethanol (96%).

Identification

Determine the infrared absorption spectrum of Amoxicillin Hydrate as directed in the potassium bromide disk method under Infrared Spectrophotometry , and compare the spectrum with the Reference Spectrum or the spectrum of Amoxicillin RS: both spectra exhibit similar intensities of absorption at the same wave numbers.

Optical rotation

+290°   to   +315°

(0.1 g calculated on the anhydrous basis, water, 100 mL, 100 mm).

Heavy metals

To 1.0 g of Amoxicillin Hydrate add 2 mL of a solution of magnesium sulfate heptahydrate (1 in 4), mix, and heat on a water bath to dryness. Carbonize the residue by gently heating. After cooling, add 1 mL of sulfuric acid, heat carefully, then heat at 500°C – 600°C to incinerate. After cooling, add 1 mL of hydrochloric acid to the residue, and heat on a water bath to dryness. Then add 10 mL of water to the residue, and heat on a water bath to dissolve. After cooling, add ammonia TS to adjust the pH to 3 – 4, and add 2 mL of dilute acetic acid. If necessary, filter, wash the residue on the filter with 10 mL of water, transfer the filtrate and washings into a Nessler tube, add water to make 50 mL, and use this solution as the test solution. Prepare the control solution as follows:

To 2.0 mL of Standard Lead Solution add 2 mL of a solution of magnesium sulfate heptahydrate (1 in 4), then proceed in the same manner as for preparation of the test solution (not more than 20 ppm).

Water:

Not less than 11.0% and not more than 15.0%

(0.1 g, volumetric titration, direct titration).

Assay

Weigh accurately an amount of Amoxicillin Hydrate and Amoxicillin RS, equivalent to about 30 mg (potency), dissolve each in a solution of boric acid (1 in 200) to make exactly 100 mL, and use these solutions as the sample solution and standard solution. Perform the test with exactly

10 mL each of the sample solution and standard solution as directed under Liquid Chromatography according to the following conditions, and calculate the peak areas, AT and AS, of amoxicillin in each solution.

Amount [µg (potency)] of amoxicillin (C16H19N3O5S)

 

= MS × AT/AS × 1000

MS = Amount [mg (potency)] of Amoxicillin RS taken

Operating conditions:

Detector:

An ultraviolet absorption photometer (wavelength: 230 nm).

Column:

A stainless steel column 4.6 mm in inside diameter and 15 cm in length, packed with octadecylsilanized silica gel for liquid chromatography (5 µm in particle diameter).

Column temperature:

A constant temperature of about 25°C.

Mobile phase:

Dissolve 1.361 g of sodium acetate trihydrate in 750 mL of water, adjust to pH 4.5 with   acetic acid, and add water to make 1000 mL. To 950 mL of this solution add 50 mL of methanol.

Flow rate:

Adjust so that the retention time of amoxicillin is about 8 minutes.

System performance:

When the procedure is run with 10 µL of the standard solution under the above operating conditions, the number of theoretical plates of the peak of amoxicillin is not less than 2500.

System repeatability:

When the test is repeated 6 times with 10 µL of the standard solution under the above operating conditions, the relative standard deviation of the peak area of amoxicillin is not more than 1.0%.

Containers and storage Containers:

Tight containers at Room temperature

Stability

≥ 2 years

Note before using Amoxicillin Product:

Do not use this medication if you are allergic to amoxicillin or to any other penicillin antibiotic, such as ampicillin, dicloxacillin, oxacillin, penicillin, and others.

Before using amoxicillin, tell your doctor if you are allergic to cephalosporins such as Omnicef, Cefzil, Ceftin, Keflex, and others. Also tell your doctor if you have asthma, liver or kidney disease, a bleeding or blood clotting disorder, mononucleosis (also called “mono”), or any type of allergy.

Amoxicillin can make birth control pills less effective. Ask your doctor about using a non-hormone method of birth control (such as a condom, diaphragm, spermicide) to prevent pregnancy while taking this medicine. Take this medication for the full prescribed length of time. Your symptoms may improve before the infection is completely cleared. Amoxicillin will not treat a viral infection such as the common cold or flu. Do not share this medication with another person, even if they have the same symptoms you have.

Antibiotic medicines can cause diarrhea. This may happen while you are taking amoxicillin, or within a few months after you stop taking it. This may be a sign of a new  infection. If you have diarrhea that is watery or bloody, stop taking this medicine and call your doctor. Do not use anti-diarrhea medicine unless your doctor tells you to.

Related Posts:

  1.    EDTA          2.  Diclofenac Sodium            3.   Vitamin “C”

Testing of Vitamin “C” in a drug

Here is the titration method for testing of Vitamin “C “in a supplement drug. It becomes more difficult to test Vitamin “C” in drug having Other vitamins like Vitamin “A “, Vitamin “E ” Vitamin B”, extracts like Ginkobiloba or Gensing and minerals like Zinc, or Seinite etc. So here is easy method to test the Vit. “C” in that drug.

PROCEEDURE: 

In the test , 1,2-diphenol-indophenol and metaphosphoric-acetic acid are used. first of all we are going to prepare both of these.

PREPARATION OF 1,2-diphenol-indophenol

Weigh 25mg of 1,2-diphenol-indolphenol in 100ml volumetric flask. add 25 ml of water and mix the weighed quantity. Now weigh 50mg of Sodium by carbonate and add in the mixture. add more 25ml of water and dissolve the reagents by continuous stirring by any mechanical means or  electromagnetic source.  and in last make the volume upto the marks using water.

PREPARATION OF Metaphosphoric Acetic-Acid

In a 100ml volumetric flask, Add 3ml of conc. phosphoric acid and 8ml of glacial acetic acid and makeup the volume upto the mark using distilled water. 

ASSAY OF VITAMIN “C”

Weigh accurately the product equivalent to 100mg of Vitamin C in 200ml volumetric flask. add 70ml of metaphosphoric acetic-acid in flask and sonicate for 30 minutes. Then makeup the volume upto the mark using distilled water. Mix the solution for 5 minutes and filter through whattman filter paper. or centrifuge some solution. take 4ml of the solution in a 100ml conical flask and add 5ml of metaphosphoric acetic acid. Now titrate with 1,2-diphenol-indophenol until rose pink color . 

each ml of 1,2-diphenol-indophenol used is equivalent to 0.136mg of Vit.C.

 

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    1. EDTA                                         2. Gentamicin Sulphate

 

 

Mohr’s Method of Precipitation Titration

MOHR’S METHOD OF DETERMINATION OF CHLORIDES BY TITRATION WITH SILVER NITRATE

Chem Pharma

is one of the oldest titration methods still in use – it was researched and published by Karl Friedrich Mohr in 1856.The idea behind this titration is very simple – chlorides are titrated with the silver nitrate solution in the presence of chromate anions. End point is signaled by the appearance of the red silver chromate.

Intense yellow color of chromate may make detection of first signs of formation of red silver chromate precipitation difficult. As some excess of silver must be added before precipitate starts to form, if concentration of titrant is below 0.1M, we may expect significant positive error. To correct for this error we can determine a blank, titrating a solution of the indicator potassium chromate with standard silver nitrate solution. To make result more realistic we can add small amount of chloride free calcium carbonate to the solution to imitate the white silver precipitate.
Solution during titration should be close to neutral. In low pH silver chromate solubility grows due to the protonation of chromate anions, in high pH silver starts to react with hydroxide anions, precipitating in form of AgOH and Ag2O. Both processes interfere with the determination accuracy.
Exactly the same approach can be used for determination of bromides. Other halides and pseudo halides, like I- and SCN-, behave very similarly in the solution, but their precipitate tends to adsorb chromate anions making end point detection difficult.

Reaction

Reaction taking place during titration is
Ag + Cl¯  →   AgCl (s)

Sample size

Assuming 0.1M titrant concentration and 50 mL burette, aliquot taken for titration should contain about 0.12-0.16 g chloride anion (3.5-4.5 millimoles).

End point detection

Before titration small amount of sodium or potassium chromate is added to the solution, making its slightly yellow in color. During titration, as long as chlorides are present, concentration of Ag is too low for silver chromate formation. Near equivalence point concentration of silver cations rapidly grows, allowing precipitation of intensively red silver chromate which signalls end point. See precipitation titration end point detection page for more detailed, quantitative discussion.

Solutions used

To perform titration we will need titrant – 0.1 M silver nitrate solution, indicator – potassium chromate solution, and some amount of distilled water to dilute sample.

Procedure

Pipette aliquot of chlorides solution into 250mL Erlenmeyer flask. Dilute with distilled water to about 100 mL. Add 1 mL of 5% potassium chromate solution. Titrate with silver nitrate solution till the first color change.

Result calculation

According to the reaction equation

Ag Cl → AgCl

silver nitrate reacts with chloride anion on the 1:1 basis. That makes calculation especially easy – when we calculate number of moles of AgNO3 used it will be already number of moles of Cl titrated. 

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if you want to read Accuracy and Precision then click on the Accuracy and Precision.

Accuracy and Precision

Accuracy
In analytical chemistry, the term ‘accuracy’ is used in relation to a chemical measurement. The International Vocabulary of Basic and General Terms in Metrology (VIM) defines accuracy of measurement as… “closeness of the agreement between the result of a measurement and a true value.” The VIM reminds us that accuracy is a “qualitative concept” and that a true value is indeterminate by nature. In theory, a true value is that value that would be obtained by a perfect measurement. Since there is no perfect measurement in analytical chemistry, we can never know the true value.
Our inability to perform perfect measurements and thereby determine true values does not mean that we have to give up the concept of accuracy. However, we must add the reality of error to our understanding. For example, lets call a measurement we make XI and give the symbol µ for the true value. We can then define the error in relation to the true value and the measured value according to the following equation:
error = XI – µ   (14.1)
We often speak of accuracy in qualitative terms such a “good,” “expected,” “poor,” and so on. However, we have the ability to make quantitative measurements. We therefore have the ability to make quantitative estimates of the error of a given measurement. Since we can estimate the error, we can also estimate the accuracy of a measurement. In addition, we can define error as the difference between the measured result and the true value as shown in equation 14.1 above. However, we cannot use equation 14.1 to calculate the exact error because we can never determine the true value. We can, however, estimate the error with the introduction of the ‘conventional true value’ which is more appropriately called either the assigned value, the best estimate of a true value, the conventional value, or the reference value. Therefore, the error can be estimated using equation 14.1 and the conventional true value.
Errors in analytical chemistry are classified as systematic (determinate) and random (indeterminate). The VIM definitions of error, systematic error, and random error follow:
Error – the result of a measurement minus a true value of the measurand.
Systematic Error – the mean that would result from an infinite number of measurements of the same measurand carried out under repeatability conditions, minus a true value of the measurand.
Random Error – the result of a measurement minus the mean that would result from an infinite number of measurements of the same measurand carried out under repeatability conditions.
A systematic error is caused by a defect in the analytical method or by an improperly functioning instrument or analyst. A procedure that suffers from a systematic error is always going to give a mean value that is different from the true value. The term ‘bias’ is sometimes used when defining and describing a systematic error. The measured value is described as being biased high or low when a systematic error is present and the calculated uncertainty of the measured value is sufficiently small to see a definite difference when a comparison of the measured value to the conventional true value is made.
Some analysts prefer the term ‘determinate’ instead of systematic because it is more descriptive in stating that this type of error can be determined. A systematic error can be estimated, but it cannot be known with certainty because the true value cannot be known. Systematic errors can therefore be avoided, i.e., they are determinate. Sources of systematic errors include spectral interferences, chemical standards, volumetric ware, and analytical balances where an improper calibration or use will result in a systematic error, i.e., a dirty glass pipette will always deliver less than the intended volume of liquid and a chemical standard that has an assigned value that is different from the true value will always bias the measurements either high or low and so on. The possibilities seem to be endless.
Precision
The term precision is used in describing the agreement of a set of results among themselves. Precision is usually expressed in terms of the deviation of a set of results from the arithmetic mean of the set (mean and standard deviation to be discussed later in this section). The student of analytical chemistry is taught – correctly – that good precision does not mean good accuracy. However, It sounds reasonable to assume otherwise.
Why doesn’t good precision mean we have good accuracy? We know from our discussion of error that there are systematic and random errors. We also know that the total error is the sum of the systematic error and random error. Since truly random error is just as likely to be negative as positive, we can reason that a measurement that has only random error is accurate to within the precision of measurement and the more precise the measurement, the better idea we have of the true value, i.e., there is no bias in the data. In the case of random error only, good precision indicates good accuracy.
Now lets add the possibility of systematic error. We know that systematic error will produce a bias in the data from the true value. This bias will be negative or positive depending upon the type and there may be several systematic errors at work. Many systematic errors can be repeated to a high degree of precision. Therefore, it follows that systematic errors prevent us from making the conclusion that good precision means good accuracy. When we go about the task of determining the accuracy of a method, we are focusing upon the identification and elimination of systematic errors. Don’t be misled by the statement that ‘good precision is an indication of good accuracy.’ Too many systematic errors can be repeated to a high degree of precision for this statement to be true.
Significant figure
There are two types of significant figures, measured and exact.
Measured Observations
As scientists we get a large amount of the numbers we report, and use in our calculations from  measured observations. In this instance a number is determined to be significant or not by the accuracy and precision of the measuring device.  With a number derived from a measurement the last digit to the right  expresses the uncertainty.  For example if you are sure that your low resolution quadrupole mass spectrometer can deliver an accurate measurements to a tenth of a mass unit then you would be justified in reporting masses to a tenth of a mass unit.  For example if one measured a mass of 110.1 u this number would contain four significant figures with the last digit expressing the uncertainty.  The uncertainty would be plus or minus 0.05 u.  Even if the instrument could spit out 10 digits passed the decimal point one should only report the significant digits.  Errors can arise in calculations if insignificant figures are used in a calculation.  If a number resulting from a measurement is used in a calculation that involves multiplication or division all significant figures should be carried through the calculation and then the result should be rounded at the end of the calculation to reflect the term used in the calculation with the fewest significant figures. For example 10.4 X 5.0 should be reported as 52 and not 52.0.  If the calculation involves addition and subtraction a different rule applies, one should preserve common decimal places of the numbers involved.  For example if two numbers obtained from a measurement are used in an addition, 10.1 1000.234 the reported number should be 1010.3. Notice that 10.1 has 3 significant figures and 1000.234 has 7 significant figures and the result of the addition has 5 significant figures.
General rules for determining the number of significant figures in a number:
A) All non-zero numbers are significant.  
B) All zeros between significant numbers are significant, for example the number 1002  has 4 significant figures.
C) A zero after the decimal point is significant when bounded by significant figures to the left, for example the number 1002.0  has 5 significant figures.
D) Zeros to the left of a significant figure and not bounded to the left by another significant figure are not significant. For example the number 0.01 only has one significant figure.
E) Numbers ending with zero(s) written without a decimal place posses an inherent ambiguity. To remove the ambiguity write the number in scientific notation. For example the number 1600000 is ambiguous as to the number of significant figures it contains, the same number written 1.600 X 10^6 obviously has four significant figures.
Several Notes:
1)  It is important to know the accuracy and precision of the measuring device one is using and it is important to report only those digits that have significance. To reiterate, your electrospray mass spectrometer may be able to spit out 10 numbers past the decimal place but you should only use the digits that have significance in reporting or in a calculation.
2) It is generally accepted that the uncertainty is plus or minus 0.5 unit at the level of the uncertainty, for example the “true value” for the number 0.003 can be described as being bounded by the numbers 0.0025 and 0.0035.  It is important to note that in some instances scientists will want to express an uncertainty that exceeds 1 at the level of the uncertainty and this should be noted explicitly in the following fashion, 0.003 ± 0.002
Exact Numbers
Exact numbers are those that are counted without ambiguity, for example the number of mass spectrometers in the lab is exactly three, or the number of cars in the parking lot is exactly four.  These numbers carry no ambiguity and can be considered to have an infinite number of significant figures.  When using these numbers in a calculation the restriction on reporting is borne by the measured number if any.

Methods of Minimizing Errors

Minimizing Systematic Error
Systematic error can be difficult to identify and correct. Given a particular experimental procedure and setup, it doesn’t matter how many times you repeat and average your measurements; the error remains unchanged. No statistical analysis of the data set will eliminate a systematic error, or even alert you to its presence. Systematic error can be located and minimized with careful analysis and design of the test conditions and procedure; by comparing your results to other results obtained independently, using different equipment or techniques; or by trying out an experimental procedure on a known reference value, and adjusting the procedure until the desired result is obtained (this is called calibration). A few items to consider:
What are the characteristics of your test equipment, and of the item you are testing? Under what conditions will the instrument distort or change the physical quantity you are trying to measure? For example, a voltmeter seems straightforward enough. You hook it up to two points in a circuit and it gives you the voltage between them. Under conditions of very low current or high voltage, however, the voltmeter itself becomes a significant part of the circuit, and the measured voltage may be significantly altered. Similarly, a large temperature probe touched to a small object may significantly affect its temperature, and distort the reading.
Check that any equations or computer programs you are using to process data behave in the way you expect. Sometimes it is wise to try a program out on a set of values for which the correct results are known in advance, much like the calibration of equipment described below.
It is unusual to make a direct measurement of the quantity you are interested in. Most often, you will be making measurements of a related physical quantity, often several times removed, and at each stage some kind of assumption must be made about the relationship between the data you obtain and the quantity you are actually trying to measure. Sometimes this is a straightforward conversion process; other cases may be more subtle. For example, gluing on a strain gauge is a common way to measure the strain (amount of stretch) in a machine part. However, a typical strain gauge gives the average strain along one axis in one particular small area. If it is installed at an angle to the actual strain, or if there is significant strain along more than one axis, the reading from the gauge can be misleading unless properly interpreted.
Calibration: Sometimes systematic error can be tracked down by comparing the results of your experiment to someone else’s results, or to results from a theoretical model. However, it may not be clear which of the sets of data is accurate. Calibration, when feasible, is the most reliable way to reduce systematic errors. To calibrate your experimental procedure, you perform it upon a reference quantity for which the correct result is already known. When possible, calibrate the whole apparatus and procedure in one test, on a known quantity similar in size and type to your unknown quantities.
Methods of minimization –
Gross errors cannot be completely eliminated, but can be minimized by taking proper care in reading and recording of the measurement parameter. One should, therefore, not be completely dependent on a single reading
Instrumental Systematic errors can be avoided by
a. selecting a suitable instrument for the particular measurement applications
b. applying correction factors after determining the amount of instrumental error
c. calibrating the instrument against a standard
Environmental Systematic errors can be avoided by air conditioning, hermetically sealing certain components in the instruments, and using magnetic shields
Observational Systematic errors can be avoided by concentrating on one particular measurement process at a time. Clearing out the area where the instrument is placed will also help the observer focus
Random errors can be treated mathematically using laws of probability. The idea is to repeat the measurement to gain high precision.

Pharmaceutical error and their types

Pharmaceutical Errors


Pharmaceutical mistakes cause more than one million serious injuries or deaths in the United States each year. Pharmaceutical errors are generally preventable, and they can result in a type of medical malpractice lawsuit. A pharmaceutical error can happen at any point in the prescription process from the time the medication is picked to the time the medication is dispensed. Most often, the error is by a nurse or doctor, but at times a pharmacist makes a mistake in filling or dispensing the prescription. Some errors happen at retail chain drug stores and prescription mail order houses.
The Food and Drug Administration (FDA) reviews medication error reports from drug manufacturers and MedWatch. According to the FDA, the most common error resulting in a fatality was the administration of an improper dose of medicine. These accounted for 41% of fatal medication errors, whereas giving the wrong drug or using an improper type of administration resulted in 16% of medication errors.


Preventing Pharmaceutical Errors


It is important for patients to pay close attention to what their doctor or pharmacist tells them about the drug they are taking, the correct dosage, and any dangerous side effects. A patient should ask questions if there is any aspect of the instructions that he or she does not understand. Patients should tell doctors the names of all prescription drugs, over-the-counter pharmaceuticals, and herbal or vitamin supplements they are taking to avoid potentially dangerous interactions between pharmaceuticals.
The Division of Medication Error Prevention and Analysis (DMEPA) reviews reports of medication errors, defined as any preventable event that could lead to inappropriate medication use or patient harm. The error may arise when the wrong pharmaceutical or the wrong dose is prescribed or instructed on the label, or when the pharmaceutical interacts improperly with other drugs.


Recover Damages for Medication Errors


A bad reaction to a medication is not necessarily a pharmaceutical error. Instead, the error must be preventable to be actionable. A pharmaceutical error must also be the actual and proximate cause of a real injury to be actionable. A patient cannot sue for a pharmaceutical error that does not result in any actual harm.
Doctors must understand their patients’ conditions in order to avoid complications or dangerous drug interactions. A doctor owes a duty to advise a patient of any drug risks so that an informed decision can be made. When a doctor fails to relay a warning to a patient, he or she will have responsibility for the error. Similarly, a doctor can also be held liable for prescribing the wrong medication, prescribing the wrong dose, or failing to notice that a patient has an allergy to an ingredient in the medication.
A patient who suffers an injury from a pharmaceutical error also can bring a medical malpractice case against a nurse, pharmacist, or hospital that makes a mistake in filling or dispensing the medication. When a pharmacist gives the wrong instructions to a patient, dispenses the wrong medication, or mixes medications that should not be mixed, he or she also can be held liable for malpractice.
Among the damages that a plaintiff may recover are past and future medical expenses, lost earnings, loss of enjoyment, pain and suffering, and loss of consortium. Depending on the state, a plaintiff’s noneconomic damages may be capped by tort reform laws. If a patient dies due to a pharmaceutical error, his or her loved ones may be able to pursue a wrongful death lawsuit.


Classification of Errors:


Errors are classified in two types – Systemic (Determinate) and Random (Indeterminate) errors


Systemic (Determinate) errors:


Errors which can be avoided or whose magnitude can be determined is called as systemic errors. It can be determinable and presumably can be either avoided or corrected. Systemic errors further classified as
Operational and personal errorInstrumental errorErrors of methodAdditive or proportional error


Operational and personal error:


Errors for which the individual analyst is responsible and are not connected with the method or procedure is called as personal errors e.g. unable to judge color change
When errors occur during operation is called as operational error e.g. transfers of solution, effervescence, incomplete drying, underweighting of precipitates, overweighing of precipitates, and insufficient cooling of precipitates. These errors are physical in nature and occur when sound analytical techniques is not followed


Instrumental and Reagent errors:


Errors occur due to faulty instrument or reagent containing impurities e.g. un-calibrated weights, un-calibrated burette, pipette and measuring flasks.


Errors of Method:


When errors occur due to method, it is difficult to correct. In gravimetric analysis, error occurs due to Insolubility of precipitates, co-precipitates, post-precipitates, decomposition, and volatilization.
In titrimetric analysis errors occur due to failure of reaction, side reaction, reaction of substance other than the constituent being determined, difference between observed end point and the stoichiometric equivalence point of a reaction.


Additive or proportional errors:


Additive error does not depend on constituent present in the determination e.g. loss in weight of a crucible in which a precipitate is ignited.
Proportional error depends on the amount of the constituent e.g. impurities in standard compound.


Random Errors:
It occurs accidentally or randomly so called as indeterminate or accidental or random error. Analyst has no control in this error. It follows a random distribution and a mathematical law of probability can be applied.

Factors of Raw Material (Active)

Here is the list of factors for some raw material in B.P and U.S.P.

By using these factors you can remove unwanted chemical groups from active and effective one. According to your label claim and raw material. I explain, let one has Lincomycin HCl and label claim for drug is only lincomycin then one should remove the HCl group or in other words, He should add so much quantity to manufacture a batch that the active Lincomycin should gave 100% assay when compared to B.P or U.S.P. Reference standard Lincomycin.

For that reason here is the list of Raw Material factors that should be multiplied with the required quantity of raw material to fulfill the requirements of active present in raw material.

Sr. NoProduct NameMolecular WeightFactor
1Atorvastatin Calcium Trihydrate 1209.421.0843
Atorvastatin1115.34
2Azithromycin Dihydrate7851.0481
Azithromycin749
3Ciprofloxacin HCl Monohydrate 385.521.1646
Ciprofloxacin331.02
4Cetirizine Dihydrochloride 461.821.1878
Cetirizine370.38
5Cefixime Trihydrate 507.51.1192
Cefixime453.45
6Calcium Acetate 158.663.9479
Calcium40.07
7Cephradine Monohydrate 367.431.0516
Cephradine349.41
8Escitalopram Oxalate414.41.2774
Escitalopram324.39
9Esomeprazole Mg.Trihydrate 762.21.1137
Esomeprazole713.1
10Iron III Hydroxide Polymaltos Complex449.163.04
Elemental Iron147.75
11Levofloxacin Hemihydrate 370.381.0249
Levofloxacin 361.38
12Montelukast Sodium 608.171.0392
Montelukast 585.17
13Naproxen Sodium252.231.1003
Naproxen 229.23
14Pantoprazole Sodium Sesquihydrate432.41.1306
Pantoprazole382.4
15Lincomycin HCl461.011.134
Lincomycin406.51
16Gentamicin Sulphate Nlt 590 µg/mg1.6949
Gentamicin1000 µg/mg
17Thiamine HCl 337.31.1213
Thiamine300.8
18Pyridoxine HCl 205.61.2158
Pyridoxine 169.1

 

Gentamicin Sulfate

Gentamicin Sulfate

ABOUT:

Gentamicin Sulfate is the sulfate of a mixture of aminoglycoside substances having antibacterial activity produced by the growth of Micromonospora purpurea or Micromonospora echinospora.

PHYSICAL APPEARANCE:

Gentamicin Sulfate occurs as a white to light yellowish white powder. It is highly hygroscopic.

CHEMICAL FORMULA:

C21H43N5O7. xH2SO4

CHEMICAL STRUCTURE:

Gentamicin Sulfate
Gentamicin Sulfate

MOLECULAR WEIGHT:

477.60

IUPAC NAME:

(6R)-2-Amino-2,3,4,6-tetradeoxy-6-methylamino-6-methyl-α-D-erythrohexopyranosyl-(1→4)-[3-deoxy-4-C-methyl-3-methylamino-β-L-arabinopyranosyl-(1→6)]-2-deoxy-Dstreptamine sulfate

CONTENTS:

It contains not less than 590 mg (potency) and not more than 775 mg (potency) per mg, calculated on the dried basis. The potency of Gentamicin Sulfate is expressed as mass (potency) of gentamicin C1

SOLUBILITY:

  • Soluble in water.
  • Typically insoluble in ethanol. (96%)

IDENTIFICATION BY PPT. FORMATION:

Dissolve 50 mg of Gentamicin Sulfate in 5 mL of water, and add 0.5 mL of barium chloride TS: a white precipitate is formed.

COLOR OF SOLUTION:

Dissolve 1.0g of Gentamicin Sulfate in 10 mL of water, the solution is clear and colorless to pale yellow.

IDENTIFICATION BY THIN LAYER CHROMATOGRAPHY:

Dissolve 50 mg each of Gentamicin Sulfate and Gentamicin Sulfate Reference Standard in 10 mL of water, and use both of these solutions as the sample solution and standard solution. Perform the test with these solutions as directed under thin layer-Chromatography. Spot 20 µL of the sample solution and standard solution on a plate of silica gel for thin layer-Chromatography. Separately, shake a mixture of chloroform, ammonia solution and methanol in ration of (2:1:1) in a separator, and allow the mixture to stand for more than 1 hour. To 20 mL of the lower layer so obtained add 0.5 mL of methanol, and use this as the developing solvent. Develop the plate with the developing solvent to a distance of about 17cm in a developing container with a cover, having an opening of about 20 mm2, and without putting a filter paper in the container, and air-dry the plate. Allow the plate to stand in iodine vapors: three principal spots obtained from the sample solution are the same with the corresponding spots obtained from the standard solution in color tone and the Rf value, respectively.

pH:

The pH of a solution obtained by dissolving 400 mg of Gentamicin Sulfate in 10 mL of water is between 3.5 and 5.5

LOSS ON DRYING:

Not more than 18.0% when 0.15g of Gentamicin Sulfate at pressure not exceeding 0.67 kPa and temperature 110°C for 3 hours. Handle the sample avoiding absorption of moisture.

RESIDUE ON IGNITION:

Should be not more than 1.0% when 1.0 gram is ignited.

SPECIFIC OPTICAL ROTATION:

+107°   to   +121° When 100mg of Gentamicin Sulfate is dissolved in 10ml of water.

QUANTITATIVE ASSAY (BIO-ASSAY):

Perform the test according to the Cylinder-plate method as directed under Microbial Assay for Antibiotics according to the following conditions.

Test organism Staphylococcus epidermidis ATCC

Agar media for seed and base layer

  • Glucose 1.0 g
  • Peptone 6.0 g
  • Meat extract 1.5 g
  • Yeast extract 3.0 g
  • Sodium chloride 10.0 g
  • Agar 15.0 g
  • Water 1000 mL

Mix all the ingredients, and sterilize. Adjust the pH of the solution so that it will be 7.8 to 8.0 after sterilization.

Agar medium for transferring test organisms.

Use the medium Agar media for seed and base layer in Medium for other organisms under Agar media for transferring test organisms.

Standard solutions

Weigh accurately an amount of Gentamicin Sulfate Reference Standard, equivalent to about 25 mg (potency), dissolve in 0.1 mol/L phosphate buffer solution (pH 8.0) to make exactly 25 mL, and use this solution as the standard stock solution. Keep the standard stock solution at 15°C or lower, and use within 30 days. Take exactly a suitable amount of the standard stock solution before use, add 0.1 mol/L phosphate buffer solution (pH 8.0) to make solutions so that each mL contains 4 mg (potency) and 1 mg (potency), and use these solutions as the high concentration standard solution and the low concentration standard solution, respectively.

Sample solutions

Weigh accurately an amount of Gentamicin Sulfate, equivalent to about 25 mg (potency), and dissolve in 0.1 mol/L phosphate buffer solution (pH 8.0) to make exactly 25 mL. Take exactly a suitable amount of this solution, add 0.1 mol/L phosphate buffer solution (pH 8.0) to make solutions so that each mL contains 4 mg (potency) and 1 mg (potency), and use these solutions as the high concentration sample solution and the low concentration sample solution, respectively.

STORAGE CONDITIONS:

It should be stored in tight and air-free containers and should be keep away from moisture area.

REFERENCES:

Japan Pharmacopia (JP XVII) Official monographs Page 983.

United State Pharmacopia (USP 41) Page 938.

Diclofenac Sodium

Diclofenac Sodium

DESCRIPTION:

Diclofenac Sodium is white or slightly yellowish, slightly hygroscopic, crystalline powder.

CHEMICAL FORMULA:

C14H10Cl2NNaO2

CHEMICAL STRUCTURE:

Diclofenac Sodium
Diclofenac Sodium

MOLECULAR WEIGHT:

318.1 Dalton

USE AS:

Cyclo-oxygenase inhibitor; analgesic; anti-inflammatory.

IUPAC NAME:

Sodium [2-[(2,6-dichlorophenyl)amino]phenyl]acetate.

CONTENTS:

It contains not less than 99.0% and not more than 101.0% of C14H10Cl2NNaO2.

SOLUBILITY:

  • Sparingly soluble in water.
  • Freely soluble in Methanol.
  • Soluble in ethanol.
  • Slightly Soluble in acetone.

MELTING POINT:

Determine the melting point of sample by using M.P instrument. It decomposes at 280°C.

IDENTIFICATION BY FTIR SPECTROPHOTOMETER:

Measure the FTIR spectra of sample and compare with standard.

IDENTIFICATION BY SODIUM REACTION:

Dissolve 60mg in 0.5mL of methanol and add 0.5 mL of water R. The solution gives reaction of sodium.

IDENTIFICATION BY COLOR OF SOLUTION:

Dissolve 1.25 gm in 25 mL methanol. And check its color & measure absorbance at 440 nm its absorbance should not be greater than 0.05

pH:

Dissolve 1.0 gm in Distilled water & dilute to 100ml and determine the pH. It should be in between 7.5 to 9.0.

LOSS ON DRYING:

Take 1.0gm of sample & dry in oven at 105-110oC for 3.0 hours. It should not be greater than 0.5%.

QUANTITATIVE ASSAY: (By Non-Aqueous TITRATION)

Dissolve 450 mg of Diclofenac Sodium in 25mL Glacial acetic acid. Add 2 drops of crystal violet indicator. Titrate with 0.1N Perchloric acid till change in color of indicator. If necessary, carry out blank titration.

Each ml of 0.1N HClO4 is equivalent to 31.81 mg of C14H10Cl2NNaO2.

CALCULATIONS:

Calculate the Percentage of Diclofenac Sodium by using following Expression.

%age assay = ((R x 31.81) /  (W-(100-X)) x 100

Where

R = Reading at Burette (Vol. of 0.1N HClO4)

W = Weight of sample taken

X = Water contents

STORAGE CONDITION:

It should be packed in airtight containers. Containers should not be transparent to light.

REFERENCE:

British Pharmacopia 2016. Volume-I, Page 740