Page 54 - Pharmaceutical Solution for Pharma Analysis

Application No.M272
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MS（Scan） FID

1, 1-Dichloroethene 1, 1, 1-Trichloroethane Carbon Tetrachloride Benzene 1, 2-Dichloroethane

3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0

Fig. 5 Chromatograms of Class 1 System Suitability Solution

To check the mass spectra of the peaks detected by FID, Table 2 Signal-to-Noise Ratio in Class 1 Standard Solution and
the peak retention times in chromatograms obtained by System Suitability Solution
FID and MS must match as closely as possible. Looking Solution for system
at Fig. 2 to 4 show all the peak retention times are lined Compound Standard solution suitability test
up, from the earliest to the latest constituent. 1, 1-Dichloroethene 221.9 141.4
When using a detector splitting system, the two 1, 1, 1-Trichloroethane 117.6 82.2
detectors must detect the same peaks detected by Carbon tetrachloride 10.2 7.6
normal gas chromatography. In other words, detector Benzene 106.3 56.8
splitting systems are expected to have the equivalent 1, 2-Dichloroethane 26.4 14.2
system performance as a normal analytical system.
Procedure A in USP <467> states the two items below
concerning system suitability. We attempted to confirm
the two items below for the detector splitting system,
and for the repeatability of class 1 standard solution
analysis. Table 3 Repeatability in Class 1 Standard Solution (n=6)
Compound Relative standard deviation (%)
(1) Detector confirmation 1, 1-Dichloroethene 1.6
The S/N ratio of 1, 1, 1-trichloroethane in class 1 1, 1, 1-Trichloroethane 2.2
standard solution is 5 or higher; the S/N ratio of each Carbon tetrachloride 1.8
peak in class 1 system suitability solution is 3 or higher. Benzene 3.5
1, 2-Dichloroethane 2.9
(2) System performance
The peak resolution between acetonitrile and
dichloromethane in class 2 standard solution is 1.0 or
higher.

The results (FID S/N ratios) of analyzing class 1 standard
solution and class 1 system suitability solution with the
detector splitting system are shown in Table 2, and the
repeatability results (FID repeatability) of analyzing class
1 standard solution are shown in Table 3. These results
show the detector splitting system meets the
performance required of a standard system. The peak
resolution of acetonitrile and dichloromethane in class 2
standard solution was 2.37, showing this system is also
suitable in terms of resolution.