Page 99 - Application Handbook - Liquid Chromatography

Application No.L466
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Table 2 Results of USP System Suitability Test Using Duloxetine
(Fig. 1 (b) Prominence-i) mV
1500
System Suitability Requirements Criteria Observed Result
Resolution Between Duloxetine and 1000 Escitalopram
Duloxetine Related Compound F ≥ 1.5 4.2 PASS
Symmetry Factor for Duloxetine ≤ 1.5 1.3 PASS 500
Peak area %RSD for Duloxetine ≤ 1.0 0.17 PASS
0

n Analysis of Impurities of Escitalopram Oxalate mV
12.5 Escitalopram
Escitalopram oxalate is used as a selective serotonin
reuptake inhibitor (SSRI). We conducted measurement of a 10.0
standard solution of escitalopram oxalate (0.5 mg/mL) B
using the analytical conditions shown in Table 3, as 7.5 (a) D
specified in the USP . Fig. 3 shows the chromatogram C E
3)
acquired using the Prominence-i in the upper, single 5.0 A
chromatogram trace, and the expanded views of the 2.5 (b)
chromatograms acquired using (a) another company's LC
system above, and that acquired using the (b) 0
Prominence-i below, in the lower, dual chromatogram
trace. 0 10 20 30 40 min
Similarly, Fig. 4 shows the chromatogram acquired using Fig. 3 Chromatograms of Escitalopram Oxalate
the Prominence-i in the upper, single chromatogram trace, Upper: Prominence-i
while in the lower, dual chromatogram trace, expanded Lower: Expanded Chromatograms by
views of the chromatogram obtained using the (a) LC-2010 (a) another Company's LC System, (b) Prominence-i
in the upper of the two traces, and that acquired using the
(b) Prominence-i with the delay volume-compatible system mV
kit option. From Fig. 3 and 4, it is clear that the 1500
Prominence-i has separation compatibility with the other
company's LC system and LC-2010 system. 1000 Escitalopram
In addition, from the results of system suitability testing
(Fig. 4 (b) Prominence-i (using the delay volume- 500
compatible system kit option)) using the system suitability
solution of Escitalopram oxalate, it is clear that the system 0
suitability was satisfied for all items, as shown in Table 4.
mV
12.5 Escitalopram
Table 3 Analytical Conditions
10.0
Column : Shim-pack VP-ODS (250 mm L. × 4.6 mm I.D., 5 µm) B
Flowrate : 1.0 mL/min *2.0 mL/min (45 - 60 min) 7.5 (a)
Mobile Phase : A) Acetonitrile / 25 mmol/L Phosphate (Potassium) D E
Buffer (pH 3.0) (1/9) C
B) Acetonitrile / 25 mmol/L Phosphate (Potassium) 5.0
Buffer (pH 3.0) (13/7)
Time Program : B. Conc. 5 % (0 min) → 35 % (35 min) → 100 % (45 - 60 min) 2.5 (b)
→ 5 % (60.1 - 68 min)
Column Temp. : 45 °C 0
Injection Volume : 20 µL
Detection : UV 237 nm 0 10 20 30 40 min
Fig. 4 Chromatograms of Escitalopram Oxalate
Upper: Prominence-i (with delay volume-compatible system kit)
Table 4 Results of USP System Suitability Test Using Escitalopram Lower: Expanded Chromatograms by (a) LC-2010,
(Fig. 4 (b) Prominence-i (with Delay Volume-Compatible (b) Prominence-i (with delay volume-compatible system kit)
System Kit))
System Suitability Requirements Criteria Observed Result [References]
1) Revision to "Cautions in Usage,"
Symmetry Factor for Escitalopram 0.8-3 2.9 PASS
Notification No. 329001 by Department of Food Safety,
Peak Area %RSD for Escitalopram ≤ 2.0 0.067 PASS Pharmaceutical and Food Safety Bureau, Japanese Ministry of
Health, Labour and Welfare (March 29, 2013)
2) Second Supplement to U.S. Pharmacopeia 35-NF 30, 2012
- Official Monographs "Duloxetine Hydrochloride"
3) U.S. Pharmacopeia 35-NF 30, 2012
- General Chapters <621>
- Official Monographs "Escitalopram Oxalate"

First Edition: Aug. 2014

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