Page 55 - Pharmaceutical Solution for Pharma Analysis

Application No.M272
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The results (chromatograms) of analyzing active Though its peak strength is smaller than that observed
pharmaceutical ingredients in the detector splitting in the standard solution, a peak was also detected at
system are shown in Fig. 6, and the mass spectra of the elution position of o-xylene (c). Checking the mass
detected peaks are shown in Fig. 7 to 9. Peaks a and b, spectrum of this peak (Fig. 9) showed it differed from
based on their respective mass spectra (Fig. 7 and 8), the mass spectrum of xylene (peak d, Fig. 10), and was
were estimated to be ethyl acetate and butanol. Both estimated to be dibutyl ether.
these constituents are low toxicity class 3 solvents.

Class1 Standard
(FID)

5.0 10.0 15.0 20.0 25.0 d 30.0 35.0
Class2A Standard
(FID)

5.0 10.0 15.0 20.0 25.0 30.0 35.0
Class2B Standard
(FID)

5.0 10.0 15.0 20.0 25.0 30.0 Test (FID) 35.0
c
b
a

5.0 10.0 15.0 20.0 25.0 30.0 Test (MS) 35.0

Fig. 6 Chromatograms of Standard Solutions and Test Solutions
100 43.0 Ethyl acetate 100 57.0 Dibutylether

50 29.0 50
61.0 41.0 87.1
0 88.1 0 73.1 130.2
50 100 150 200 250 50 100 150 200 250
Fig. 7 Mass Spectrum of Peak a Fig. 9 Mass Spectrum of Peak c
100 56.0 100 91.1
31.0 n-Butanol o-Xylene
106.2
50 50
51.0 77.0
0 0
50 100 150 200 250 50 100 150 200 250
Fig. 8 Mass Spectrum of Peak b Fig. 10 Mass Spectrum of Peak d
n Conclusion
An FID and MS detector splitting system obtains FID and MS data simultaneously in a single analysis, and can be used
as a simpler method of confirming constituent identity. This system shows promise for use in residual solvent testing of
pharmaceuticals.
Note: Reference USP <467>
This data was obtained by a method that does not conform to the pharmacopoeia, as analytical conditions based on USP <467> was modified before use.
First Edition: Jul. 2016
For Research Use Only. Not for use in diagnostic procedure.
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