Ensure all the connections of the
instrument are proper before use.
Open carrier gas used for TOC (Zero air cylinder) with cylinder pressure and gas line pressure maintained at 4-6 Kg/cm2.
The pressure of the carrier gas i.e. Zero air should be 2 Kg/cm2 (200 kpa) and flow should be 150 ml/min. Adjust if necessary by opening the front door and adjusting gas pressure controller and mass flow controller.
Ensure level of the water in the humidifier should be kept between two marks shown on the bottle i.e. between (High and Low mark).
Get the raw data (printout) of the analysis checked.
Open carrier gas used for TOC (Zero air cylinder) with cylinder pressure and gas line pressure maintained at 4-6 Kg/cm2.
The pressure of the carrier gas i.e. Zero air should be 2 Kg/cm2 (200 kpa) and flow should be 150 ml/min. Adjust if necessary by opening the front door and adjusting gas pressure controller and mass flow controller.
Ensure level of the water in the humidifier should be kept between two marks shown on the bottle i.e. between (High and Low mark).
Get the raw data (printout) of the analysis checked.
· Disintegration test Apparatus
Ensure that
the instruments in calibrated condition before use.
Ensure all
the connections of the instrument are proper before use.
Ensure, the
bath is filled with water up to the level marked (without beakers)
Set the
temperature to 37oC unless otherwise specified.
Clean the basket rack assembly,
beakers, and discs after use.
· Friabilator
Ensure that
the instrument s in calibrated condition before use.
Ensure all
the connections of the instrument are proper before use.
For tablets with a unit weight equal to or less than 650 mg,
take a sample of whole tablets corresponding as near as possible to 6.5 g. For
tablets with a unit weight of more than 650 mg, take a sample of 10 whole tablets.
The tablets should be carefully dedusted prior to testing.
Accurately weigh the tablet sample, and place the tablets in
the drum. After testing remove the tablets. Remove any loose dust from the
tablets as before, and accurately weigh.
After conducting friability test,
weighing of the tablets shall be done within 15 minutes.
· Statistical tools for evaluation of data
Mean and Standard deviation:
Mean
(arithmetic mean) is given by the formula
X1 + x2 + x3 +
……. xn-1 + xn
X =
---------------------------------------
n
Standard deviation (S), is given by the formula
Standard deviation (S), is given by the formula
_________________
∑ (x - x)2
∑ (x - x)2
S = -----------------
n-1
Relative
standard deviation (RSD), is given by formula
S
RSD = -------
x
Comparison of results
The
comparison of the values obtained from a set of results with either the true
value or with other sets of data makes it possible to determine whether the
analytical procedure has been accurate and / or precise, or if it is superior
to another method. There are two common method for comparing results, Student’s
t-test and the variance ratio test (F-test).
Student’s
t-test
This is the test used for small samples; its purpose is to compare the mean from a sample with some standard value and to express some level of confidence in the significance of the comparison. It is also used to test the difference between the means of two sets of data x1 and x2.
The value of t is obtained from the equation
This is the test used for small samples; its purpose is to compare the mean from a sample with some standard value and to express some level of confidence in the significance of the comparison. It is also used to test the difference between the means of two sets of data x1 and x2.
The value of t is obtained from the equation
(x- µ)
T = ----------
s
Where µ is
the true value.
F-test
This is used
to compare the precisions of two sets of data, e.g. the results of two
different analytical methods or the results from two different laboratories. It
is calculated from the equation
S2A
F = ------------------
S2B
The larger value of S is always used as the numerator, so the value of F is always greater than unity.
S2A
F = ------------------
S2B
The larger value of S is always used as the numerator, so the value of F is always greater than unity.
Comparing
the means of two samples
When a new
analytical method is being developed it is usual practice to compare the values
of the mean and precision of the new (test) method with those of an established
(reference) procedure.
The value of t when comparing two sample means x1 and x2 is given by the expression
The value of t when comparing two sample means x1 and x2 is given by the expression
x1-
x2
t = ------------------------------
Sp 1/n1 + 1/n2
Where Sp,
the pooled standard deviation, is calculated from the two sample standard
deviations S1 and S2, as follows:
(n1-1)s21 +
(n2-1)s22
Sp = --------------------------------
n1 +
n2 - 2
Note that there must not be a significant difference between the precisions of the methods. Hence the F-test is applied before using the t-test in equation.
Note that there must not be a significant difference between the precisions of the methods. Hence the F-test is applied before using the t-test in equation.
When using
instrumental methods it is often necessary to carry out a calibration procedure
by using a series of samples (standards) each having a known concentration of
the analyte to be determined. A calibration curve is constructed by measuring
the instrumental signal for each standard and plotting this response against
concentration. Provided the same experimental conditions are used for the
measurement of the standards and for the test (unknown) sample, the
concentration of the test sample may be determined from the calibration curve
by graphical interpolation.
Correlation
coefficient
To establish
whether there is a linear relationship between two variables x1 and
y1, use Pearson’s correlation coefficient r :
n∑ x1y1 -
∑x1∑y1
r =
---------------------------------------------------------
{[n∑x21 – (∑x1)2][n∑y21 –(∑y1)2]}1/2
Where n is
the number of data points.
The value of r must lie between +1
and -1; the nearer it is to ± 1, the greater the probability that a definite
linear relationship exists between the variables x and y; values close to +1
indicate positive correlation and values close to -1 indicate negative
correlation. Values of r that tend towards zero indicate that x and y are not
linearly related (they may be related in a non-linear fashion).
· Microbiology testing
Use correct
incubation period and temperature specified in the method of analysis.
Ensure that
the growth promotion test is
performed for the media to be used for analysis.
Take all
required precautions while handling the Microbiological cultures.
Ensure that
the Microscope is calibrated and working properly.
Ensure that
all the glassware's used for microbial analysis are decontaminated properly.
Culture / suspending / sub culturing
should be traceable.
· General precaution
Precautions:
Crosscheck
the exactness of instrument method / program & sequence with respect to the
method of analysis.
Crosscheck
the exactness of sequence with respect to the samples loaded in auto sampler.
Always
compare response obtained with previous data as a tool of crosscheck.
Use correct
excel sheet for calculation.
Avoid
glassware breakage. Upon breakage of any glassware intimate to your respective
supervisor so that the requirement for the same can be raised to avoid shortage
of glassware.
Keep the
allocated samples in the respective designated area during and after analysis
duly labeled.
Record the
temperature and humidity of the areas daily
once and intimate to immediate supervisor if any excursion is observed for more
than half an hour.
· Interpretation
Interpretation
should be aligned with the requirements in the method of analysis.
Interpretation should be done by considering the category of the method e.g. Related substances, assay etc.
Do not use manual integration events for quantification method unless otherwise specified in the method.
Interpretation should be done by considering the category of the method e.g. Related substances, assay etc.
Do not use manual integration events for quantification method unless otherwise specified in the method.
Compare the
chromatographic data with specimen chromatogram.
If the
results are not as per trend then inform immediately to immediate supervisor.
· Records & Reports
Record the
values & results online.
Check the
entered values & figures for correctness online.
Calculate
the results using correct formula (as per method of analysis) &
recheck once online.
Do not
overwrite the wrong entry. Cross it out with a line permitting the reading of
original entry. Clearly write the correct entry near the cross out & sign
the data along with the date on which correction is made.
Do not leave
the blank spaces. Draw a line across the page from left to right.
All the
document entries shall be made with indelible black ink in clear & legible
hand writing.
Columns or
rows not required shall be marked as ‘N.A.’ or ‘—’.
Validate
excel sheet whenever required for calculation of results of CU/BU & dissolution
(Profile/ Single point).
Use correct
path of validated excel sheet for calculation of results.
Ensure that
the usage and consumption entry is made in the respective instrument and column
log book and working standard log book respectively.
Ensure that
the respective index is updated when any SOP/ Document is created / revised.
