Validation: The validation was performed for fallowing method for these analytical parameters System suitability, Accuracy, Precision, Linearity, LOQ, LOD, Robustness.
a) Accuracy The closeness of agreement between the value, which are accepted either as a conventional true value or an accepted reference value and the value found. Accuracy is represented and determined by recovery studies.
b) Precision The precision of an analytical procedure expresses the closeness of agreement between a series of measurement obtained from multiple sampling of the homogenous sample under the prescribed condition.
c) Linearity: The linearity of an analytical procedure is its ability to obtain test results, which are directly proportional to the concentration …show more content…
The detection limit (LOD) may be expressed as LOD = 3.3
e) Quantitation Limit The Quantitation limit of an analytical procedure is the lowest amount of analyte in a sample, which can be quantitatively determined with suitable precision and accuracy. Quantitation Limit (LOD) may be expressed as LOQ = 10 S
Where
= the standard deviation of the response S = the slope of the calibration curve (of the analyte)
f) Ruggedness Method ruggedness is defined as the reproducibility of results when the method is performed under actual use includes different analysts, laboratories, columns, instruments, sources of reagents, chemicals, solvents and so on. Method ruggedness may not be known when a method is first developed, but insight is obtained during subsequent use of that method.
Results and Discussion Chromatogram of DAPA and SAXA Got chromatogram at RT’s of 4.707 min for Dapagliflozin and 6.684min for Saxagliptin.
S.NO Name of the peak Retention time(min)
1 Dapagliflozin 4.707
2 Saxagliptin …show more content…
No Conc.(μg/ml) Peak area (n=6) % Assay MET EMPA DAPA SAXA DAPA SAXA
1 10 10 633495 1202110 98.88 98.6
2 10 10 635992 1203700 99.40 99.02
3 10 10 639828 1201851 99.30 98.12
4 10 10 639098 1202255 100.53 98.31
5 10 10 648289 1203283 98.28 98.81
6 10 10 631322 1202349 99.278 98.36
MEAN 637312 122854 99.28 98048
SD 2.12 1.61 0.827 0.68
% RSD 0.0891 0.1358 0.13 0.35
System precision for Dapagliflozin and Saxagliptin
S. No Conc.(μg/ml) Peak area (n=6) % Assay DAPA SAXA DAPA SAXA DAPA SAXA
1 10 10 674753 1218805 98.66 99.95
2 10 10 674261 1214014 99.30 100.24
3 10 10 675298 1215474 101.53 100.06
4 10 10 679221 1227655 100.53 99.30
5 10 10 688636 1267019 99.98 100.00
6 10 10 674627 121401 98.06 100.02
Mean
SD 678433 6031.125 122124.07 22124.07 100.61
0.31 100.00 1.1076
% RSD 0.888 1.80007 0.30 1.10
System
a) Accuracy The closeness of agreement between the value, which are accepted either as a conventional true value or an accepted reference value and the value found. Accuracy is represented and determined by recovery studies.
b) Precision The precision of an analytical procedure expresses the closeness of agreement between a series of measurement obtained from multiple sampling of the homogenous sample under the prescribed condition.
c) Linearity: The linearity of an analytical procedure is its ability to obtain test results, which are directly proportional to the concentration …show more content…
The detection limit (LOD) may be expressed as LOD = 3.3
e) Quantitation Limit The Quantitation limit of an analytical procedure is the lowest amount of analyte in a sample, which can be quantitatively determined with suitable precision and accuracy. Quantitation Limit (LOD) may be expressed as LOQ = 10 S
Where
= the standard deviation of the response S = the slope of the calibration curve (of the analyte)
f) Ruggedness Method ruggedness is defined as the reproducibility of results when the method is performed under actual use includes different analysts, laboratories, columns, instruments, sources of reagents, chemicals, solvents and so on. Method ruggedness may not be known when a method is first developed, but insight is obtained during subsequent use of that method.
Results and Discussion Chromatogram of DAPA and SAXA Got chromatogram at RT’s of 4.707 min for Dapagliflozin and 6.684min for Saxagliptin.
S.NO Name of the peak Retention time(min)
1 Dapagliflozin 4.707
2 Saxagliptin …show more content…
No Conc.(μg/ml) Peak area (n=6) % Assay MET EMPA DAPA SAXA DAPA SAXA
1 10 10 633495 1202110 98.88 98.6
2 10 10 635992 1203700 99.40 99.02
3 10 10 639828 1201851 99.30 98.12
4 10 10 639098 1202255 100.53 98.31
5 10 10 648289 1203283 98.28 98.81
6 10 10 631322 1202349 99.278 98.36
MEAN 637312 122854 99.28 98048
SD 2.12 1.61 0.827 0.68
% RSD 0.0891 0.1358 0.13 0.35
System precision for Dapagliflozin and Saxagliptin
S. No Conc.(μg/ml) Peak area (n=6) % Assay DAPA SAXA DAPA SAXA DAPA SAXA
1 10 10 674753 1218805 98.66 99.95
2 10 10 674261 1214014 99.30 100.24
3 10 10 675298 1215474 101.53 100.06
4 10 10 679221 1227655 100.53 99.30
5 10 10 688636 1267019 99.98 100.00
6 10 10 674627 121401 98.06 100.02
Mean
SD 678433 6031.125 122124.07 22124.07 100.61
0.31 100.00 1.1076
% RSD 0.888 1.80007 0.30 1.10
System