Page 49 - Pharmaceutical Solution for Pharma Analysis

Application No.L489
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n Linearity n Analysis of a Pharmaceutical Excipient
Fig. 3 shows the calibration curve of mannitol analyzed Fig. 5 shows an example of analysis of a pharmaceutical
using the conditions of Table 1. The correlation excipient, consisting mainly of mannitol, using a 20 μL
coefficient over the concentration range from 1 to injection of 50 g/L sample solution. The chromatogram
2
100 g/L is R = 0.999, demonstrating excellent linearity. of the excipient is shown in the upper portion of the
figure, while an expanded view of the chromatogram is
Area (×10 ) 5 shown in the lower portion. Trace levels of other
275 substances, including sorbitol and isomalt, were also
detected in the excipient.
250 R =0.999
2
225
uRIU
1000
200
750
175 Mannitol
500
150
125 250
100 0
0.0 5.0 10.0 15.0 20.0 25.0 min
75
uRIU
50 10
9 Mannitol
25
8
0 7
0.0 25.0 50.0 75.0 100.0 Conc. (g/L)
6
Fig. 3 Linearity of Calibration Curve 5 Sorbitol
4
n Effect of Column Temperature
3
Fig. 4 shows the chromatograms obtained in analysis of 2
the four sugar alcohol standard samples using the two 1 Isomalt
column oven temperatures of 85 °C and 60 °C. The 0
upper pair of chromatograms are those of isomalt and 0.0 5.0 10.0 15.0 20.0 25.0 min
maltitol, and the lower pair, of mannitol and sorbitol.
When the column temperature is lowered to 60 °C, the Fig. 5 Chromatogram of Pharmaceutical Excipient
retention time of mannitol becomes 23 minutes, at Upper: Chromatogram
which point the system suitability requirement is no Lower: Expanded Chromatogram
longer satisfied. Reference
When analysis is conducted at a high column 1) United States Pharmacopeia, Second Supplement to USP 37–NF 32
temperature like 85 °C, it is important that the
temperature be maintained uniformly over the entire The samples used to produce this application were kindly provided
length of the column. The CTO-20AC column oven by Nihon Generic Co., Ltd.
used in this analysis is equipped with forced air
circulation, thereby permitting stable analysis even at
high temperatures.
uRIU
2 ■ Peaks
25
1. Isomalt (1)
20 2. Maltitol
1 3
15 85 ˚C 3. Isomalt (2)
10
5 60 ˚C 1 2, 3
0
0.0 2.5 5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 min
uRIU
600
4 5 ■ Peaks
500 4. Mannitol
5. Sorbitol
400
85 ˚C
300
200 4 5
100 60 ˚C
0
0.0 5.0 10.0 15.0 20.0 25.0 30.0 min
Fig. 4 Chromatograms of a Standard Mixture of Four Sugar
Alcohols (85 °C, 60 °C)
First Edition: Apr. 2015

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