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SAMPLING
Sample equal quantity from each container. Sample a minimum of 5 g from each of
the containers into individual, non-toxic, self-sealing, transparent polythene bag
bearing Sample for analysis label kept in another black self-sealing polythene bag
bearing Sample for analysis label.
QUANTITY OF COMPOSITE SAMPLE FOR ANALYSIS
10g
REANALYSIS PERIOD ##
One year
CATEGORY
Antiviral
HAZARDS AND PRECAUTIONS, IF ANY
Wear nose mask and hand gloves while sampling. Avoid inhalation or exposure to
skin and reseal the containers immediately after sampling.
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Page 1 of 10
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(S)-isopropyl-2-((S)-(((2R,3R,4R,5R)-5-(2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)-4-fluoro-3-hy
droxy-4-methyltetrahydrofuran-2-yl)methoxy)-(phenoxy)phosphorylamino)propanoate
DESCRIPTION:
A white to off white powder.
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SOLUBILITY:
Slightly soluble in water (pH 1.2-7.7), freely soluble in ethanol and acetone, soluble in
2-propanol, and insoluble in heptane.
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IDENTIFICATION:
A) <By Infrared absorption spectrophotometry>
The Infrared absorption spectrum is concordant with the spectrum obtained from
the similar preparation of Sofosbuvir Test Stands /Working Standard.
B) <By High performance liquid chromatography>
The principal peak in the chromatogram obtained with the test solution is similar in
retention time and size to the principal peak in the chromatogram obtained with
reference solution.
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WATER:
Not more than 0.50% w/w.
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2. SOLUBILITY
Dissolve 1g of accurately weighed sample to 10ml of ethanol and acetone,
respectively, check the solubility; Dissolve 1g of accurately weighed sample to 30ml
of 2-propanol, check the solubility; Dissolve 0.1g of accurately weighed SOF to 100ml
of water, check the solubility; Dissolve 0.1g of accurately weighed SOF to 1000ml of
heptane, check the solubility.
Reporting: Report as Complies/Does not Comply.
3. IDENTIFICATION
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4.
WATER
5.
6.
HEAVYMETALS
7.
MELTING POINT
Reduce the substance to a very fine powder Introduce into a capillaryglass tube, a
sufficient quantity of the dry powder to form acompact column 4 to 6 mm high. Heat
the bath until the temperature is about 10 below the expected melting temperature.
the temperature to rise at a rate of about 10 per minute.
Reporting: Report as a value in .
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Methanol
Tetrahydrofuran
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Ethyl acetate
Acetic acid
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Class of solvent
Class 2
Class 2
Class 2
Class 3
Class 3
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Testing of other Class 12 and 3 residual solvents and other organic solvents is not
required since these solvents are not used during manufacturing process.
Report the same as `Complies` with remark as `Testing of other Class 12 and 3
residual solvent and other organic solvents is not required as these solvents are not
used during manufacturing process;
Instrument: A Gas chromatograph capable of temperature programming, equipped
with a capillary column, split/splitless injector, a flame ionization detector.
Chromatoaraphic conditions:
Chromatographic Conditions:
Chromatographic Column: 30m 0.53mm 3m, DB-624
Column temperature: Hold at 40for 8min, then increase at a rate of 15 per min
to 150, Further increase at a rate of 30/min to 210 and hold for 5min.
Flow rate: 5.0ml/min
Split ratio: 1:10
Carrier gas: Nitrogen
Purge flow: 3.0ml/min
Injection port temperature: 200C
Detector temperature: 250C
Injection volume: 1.0l
Reference Stock Solution I Transfer about 0.20ml of 2-pentanone, accurately
measured, to a 1000ml volumetric flask as internal standard. Dilute with a mixture
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( AT / ATI ) C S
100%
( AS / ASI ) CT
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where,
CS = the concentration of the respective analyte in the Standard solution, in mg / ml;
CT =the concentration of test solution, in mg /ml;
AT =the peak area of respective analyte in the test solution;
ATI = the peak area obtained from the internal standard in the test solution;
AS = the peak area of respective analyte in the standard solution;
ASI =the peak area obtained from the internal standard solution in the standard
solution.
Reporting: Report as a value in ppm
If no peak is observed at the expected retention time of specified solvent, then
report as "N.D".
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Chromatographic conditions:
Standard column type
C18,4.6*150mm,5 um
Detection
spectrophotometer at 260 nm.
Flow rate
1.2 ml/min
Column oven temperature
35
Injection volume
20 ul
Diluent
DMSO
Mobile phase A
0.05%TFA IN(5%MEOH)
Mobile phase B
0.05%TFA IN(95%MEOH)
Xiamen Halosyntech Co., Ltd. Page 6 of 10
0
7
15
30
35
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30
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2
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49
70
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100
100
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A CS
100%
B CT
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C18,4.6*150mm,5um
spectrophotometer at 260 nm.
1.2 ml/min
35
10 ul
0.05%TFA IN(5%MEOH)
0.05%TFA IN(95%MEOH)
Isocatic ( Mobile phase A: Mobile phase B=52:48)
About 20 min
DMSO
Weigh accurately about 25 mg of Sofosbuvir Test
Standard / Working Standard and transfer into a 25 ml
volumetric flask. Dissolve and dilute to volume with
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AW1 P
BW2
Where:
A=Peak area response of T Sofosbuvir obtained in the chromatogram of sample
solution.
B= Average peak area response of Sofosbuvir obtained in the chromatogram of
Standard solution A.
W1 = Weight of Sofosbuvir Test /Working Standard in Standard solution A in mg.
W2=Weight of Sample in mg.
P=%w/w Assay of Sofosbuvir Test Standard/Working Standard on as such basis.
If the assay values obtained are within the limit, calculate the %variation between
both the assay values using the formula:
=2X
x 100
The assay results are acceptable only if the variation is less than
Xiamen Halosyntech Co., Ltd. Page 9 of 10
2.0%.If the acceptable criteria for %variation is met, report the mean assay value
using the formula:
=
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