-Analysis of decomposition products in aspirin

by application of two-wavelength detection-

The Chromaster 5410 (UV Detector) permits two-wavelength simultaneous measurements by realtime wavelength-
switching. 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 OH

MW = 180.16 MW = 138.12
1. Acetyl salicylic acid (Aspirin) 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
7 0 .0 0
6 0 .0 0
A U

5 0 .0 0
m

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 7 .0 0 8 .0 0 9 .0 0 1 0 .0 0
Data collection interval:分400 ms

1 0 0 .0 0
9 0 .0 0
[LC conditions ]
8 0 .0 0 Aspirin Column HITACHI LaChrom C18, 5 µm
7 0 .0 0 4.6 mm I.D.×150 mm
Mobile
6 0 .0 0 Unknown
Phase 20 mM CH3COONH4/CH3OH = 80/20
A U

component 205 nm
5 0 .0 0 Flow rate 1.0 mL/min
m

4 0 .0 0 Salicylic acid Temperature 40˚ C

Detection UV 205 nm ,270 nm
3 0 .0 0 270 nm Injection vol. 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 4 .0 0 5 .0 0 6 .0 0 7 .0 0 8 .0 0 9 .0 0 1 0 .0 0
mim mm
分
9
ユ ー ザ ー 名 ： 　 S y stem プ ロ ジ ェク ト 名 ：　 w _W L_101014
レ ポ ー ト メ ソ ッド 名 ：　 カ タ ロ グ 用 10_17_2
Aspirin - Enlarged view 印 刷 日 ： 　
レ ポ ー ト メ ソ ッ ド ID ： 　 1 2 0 2 (270 nm) カ タ ロ グ 用 1 0 _ 1 7 _ 2 2_031 0 / 1 0 / 1 4
ペ ー ジ 番 号 ： 　 1 /1 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 By setting a data collection interval of 400
1 8 .0 0 Data collection interva:l: ms, peaks can be determined accurately
800 ms
1 6 .0 0 without missing peak tops.
U

1 4 .0 0
A

1 2 .0 0 Data collection interval:

m

1 0 .0 0 400 ms
8 .0 0 Optimal condition need to be set according
6 .0 0 to given S/N values.
4 .0 0
2 .0 0
0 .0 0
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

2 4 .0 0
2 2 .0 0
2 0 .0 0
Whereas minute1 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
U

simultaneous1 detection
4 .0 0 at 205 nm, micro-peaks such as decomposition products and additives can be verified at
A

the same time.1 2 .0 0

m

1 0 .0 0
8 .0 0
NOTE: These data
6 .0 0 are an example of measurement; the individual values cannot be guaranteed. Page .2
4 .0 0
2 .0 0
Hitachi-High0 .0 Technologies
0
Analysis Systems 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 1
分

ユ ー ザ ー 名 ： 　 S y stem プ ロ ジ ェク ト 名 ：　 w _W L_101014