Page 21 - Pharmaceutical Solution for Pharma Analysis

Application No. L518
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Table 2 Results of System Suitability Test
mAU
System suitability Results Judgements
requirements Conventional High speed
10
Resolution
(H2B1b and H2B1a) ≥ 3.0 5.1 4.7 PASS Diclofenac
Signal-to-noise ratio ≥ 10 40 38 PASS
(0.4 μg/mL) F
5
Symmetry factor ≤ 2.5 1.1 1.2 PASS

A
„ High Speed Analysis of Diclofenac Sodium and
Related Substances 0
Diclofenac is widely used as an antipyretic and a pain- 0.0 25.0 50.0 min
reliever. Here we introduce an example of high speed
analysis of a diclofenac sodium and related substances
based on the EP. mAU
Fig. 2 shows the resulting chromatograms of diclofenac 15
standard solution (1.0 mg/mL). Table 3 lists the analysis
*3
conditions that comply with both the testing section Diclofenac
of diclofenac sodium related substances and the 10
allowable adjustment range assigned in the EP. The F
analytical columns used in conventional analysis and
high speed analysis were both the same as those used 5
in the analysis of ivermectin. A commercially-available
reagent for system suitability testing was used as the A
reference standard. 0
In conventional analysis, the mobile phase flow rate
assigned in the EP is 1.0 mL/min. Despite adjusting the 0.0 5.0 10.0 15.0 min
flow rate to 0.8 mL/min in this research due to the column
pressure tolerance, which is within the allowable Chromatograms of Diclofenac Standard Solution
adjustment range, the obtained results meet the system Upper: Conventional Analysis Using HPLC Flow Line (Column 1)
suitability requirements (Table 4). High speed analysis also Lower: High Speed Analysis Using UHPLC Flow Line (Column 2)
passed the system suitability test. The high speed analysis
provided approximately 70 % and 40 % reductions of
analysis time and mobile phase consumption respectively <References>
while maintaining enough separation. *1 European Pharmacopoeia 8.0, 04/2009:20246
2.2.46. Chromatographic separation techniques
As demonstrated above, Nexera-i MT not only *2 European Pharmacopoeia 8.8, 04/2016:1336 "Ivermectin"
facilitated migration from conventional analysis to *3 European Pharmacopoeia 8.8, 07/2014:1002 "Diclofenac sodium"
high speed analysis but also provided results of an
equal level.

Table 3 Analytical Conditions
System : Nexera-i MT
Column 1 : Shim-pack GIST C18
(Conventional) (250 mm L, 4.6 mm I.D., 5 Pm)
Flow rate 1 : 0.8 mL/min
Column 2 : Shim-pack GIST C18
(High speed) (150 mm L, 4.6 mm I.D., 3 Pm)
Flow rate 2 : 1.4 mL/min
Mobile phase : A) Sodium phosphate buffer (pH 2.5)
B) Methanol
A/B=34/66 (v/v)
Column temp. : 25 qC
Injection volume : 20 μL
Detection : UV 254 nm

Table 4 Results of System Suitability Test
System suitability Results Judgement
requirement Conventional High speed
Resolution
(impurity F and ≥ 4.0 6.8 5.1 PASS
Diclofenac)

First Edition: Apr. 2017
For Research Use Only. Not for use in diagnostic procedure.
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