-Analysis of decomposition products in aspirin
by application of two-wavelength detectionThe Chromaster 5410 (UV Detector) permits two-wavelength simultaneous measurements by realtime wavelengthswitching. Beyond the measurement of impurities, the system provides a powerful tool for the analysis of proteins
and peptides. By setting a data capture interval of 400 ms or greater for wavelength-switching, users can
accurately detect peaks without missing any data points. The following data describes the simultaneous analysis of
aspirin and an aspirin degradation product.
[Analysis of decomposition products in an aspirin-based drug ]
Sample: Drug containing aspirin (acetyl salicylic acid)
As an important mechanism of action, aspirin reportedly suppresses the biosynthesis of prostaglandin and exhibits
analgesic, fever-lowering, and anti-inflammatory actions. As a fever-lowering analgesic drug, aspirin is widely used
both in prescription and over-the-counter drugs, and it is also contained in general common cold remedies.
CO2H
CO2H
O
O
CH3
MW = 180.16
1. Acetyl salicylic acid (Aspirin)
OH
MW = 138.12
2. Salicylic acid
In aqueous solution, aspirin is known to undergo decomposition by hydrolysis into salicylic acid, and it is
reported that the decomposition reaction is promoted at high temperatures, in alkaline solutions, and in the
presence of magnesium. (Because aspirin, even in a reagent, contains trace quantities of salicylic acid, it must
be handled with care when used as a standard compound.)
[Preparation of sample]
Ultra-deionized water, 1000 mL, was added to one tablet, and the tablet was disintegrated by ultrasound treatment.
After that, the mixture was filtered with a membrane filter and used as a sample.
[System configuration]
Chromaster 5110 pump
Chromaster 5210 AutoSampler
Chromaster 5310 Column Oven
Chromaster 5410 UV Detector
Empower2 Data Processing System
Chromaster system
Page .1
1 0 0 .0 0
9 0 .0 0
8 0 .0 0
m
A U
7 0 .0 0
6 0 .0 0
5 0 .0 0
4 0 .0 0
3 0 .0 0
2[Results
0 .0 0
of analysis]
1 0 .0 0
0 .0 0
0 .0 0
1 .0 0
2 .0 0
3 .0 0
4 .0 0
5 .0 0
6 .0 0
Data collection interval:分400 ms
7 .0 0
8 .0 0
9 .0 0
1 0 .0 0
1 0 0 .0 0
[LC conditions ]
9 0 .0 0
8 0 .0 0
Column
Aspirin
m
A U
7 0 .0 0
Unknown
component
6 0 .0 0
5 0 .0 0
Mobile
Phase
Flow rate
Temperature
Detection
Injection vol.
205 nm
Salicylic acid
4 0 .0 0
3 0 .0 0
270 nm
HITACHI LaChrom C18, 5 µm
4.6 mm I.D.×150 mm
20 mM CH3COONH4/CH3OH = 80/20
1.0 mL/min
40˚ C
UV 205 nm ,270 nm
20 µL
2 0 .0 0
1 0 .0 0
0 .0 0
0 .0 0
1 .0 0
2 .0 0
3 .0 0
m
A
U
ユ ー ザ ー 名 ： S y stem
レ ポ ー ト メ ソ ッド 名 ：　カ タ ロ グ 用 10_17_2
レ ポ ー ト メ ソ ッ ド ID ： 1 2 0 2
ペ ー ジ 番 号 ： 1 /1
4 .0 0 5 .0 0
mim mm
分
9
6 .0 0
7 .0 0
8 .0 0
9 .0 0
1 0 .0 0
プ ロ ジ ェク ト 名 ：　w _W L_101014
Aspirin - Enlarged
view 印 刷 日 ： カ タ ロ グ 用 1 0 _ 1 7 _ 2 2_031 0 / 1 0 / 1 4
(270 nm)
1 5 : 2 5 : 4 8 A s ia / T o k y o
2 4 .0 0
2 2 .0 0
2 0 .0 0
1 8 .0 0
1 6 .0 0
1 4 .0 0
1 2 .0 0
1 0 .0 0
8 .0 0
6 .0 0
4 .0 0
2 .0 0
0 .0 0
Data collection interva:l:
800 ms
By setting a data collection interval of 400
ms, peaks can be determined accurately
without missing peak tops.
Data collection interval:
400 ms
Optimal condition need to be set according
to given S/N values.
3 .9 0 4 .0 0 4 .1 0 4 .2 0 4 .3 0 4 .4 0 4 .5 0 4 .6 0 4 .7 0 4 .8 0 4 .9 0 5 .0 0
Min. 分
m
A
U
2 4 .0 0
2 2 .0 0
2 0 .0 0
Whereas minute
1 8 .0 0 peaks associated with decomposition products and additives cannot be detected accurately at
270 nm, which
1 6 .0is
0 the optimal measurement wavelength for aspirin (USP, Japan Pharmacopeia: Elution test), by
simultaneous1 detection
at 205 nm, micro-peaks such as decomposition products and additives can be verified at
4 .0 0
the same time.
1 2 .0 0
1 0 .0 0
8 .0 0
NOTE: These data
Page .2
6 .0 0 are an example of measurement; the individual values cannot be guaranteed.
4 .0 0
2 .0 0
Hitachi-High0 .0 Technologies
0
Analysis Systems
1
3 .9 0 4 .0Marketing
0 4 .1 0 4 .2 0 4 .3 0 Division,
4 .4 0 4 .5 0 4 .6 0 Marketing
4 .7 0 4 .8 0 4 .9 0 5Division
.0 0
分
ユ ー ザ ー 名 ： S y stem
プ ロ ジ ェク ト 名 ：　w _W L_101014