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Review of Analytical Methods: Hua Yin
Review of Analytical Methods: Hua Yin
Analytical Methods
Hua YIN
Outline
Mobile phase
System precision
– Assay: RSD≤ 2% for FPP, n ≥ 5 – using RS solution
RSD ≤1% for API (see table below)
Number of theoretical plates (N) and tailing factor (T) can be used as additional SSTs ,or if there are no suitable impurities for the determination of resolution
For Assay:
Rifampicine Quinone:
y = 26.198 x + 1.154
Rifampicine:
y =31.312 x + 4.963
=0.84
To review:
Chromatographic condition
– Column: size (l, Ø), stationary phase, particle size (packed column),
film thickness (capillary column)
– Carrier gas: helium or nitrogen
– Flow rate
– Injection volume and split volume: e.g. 1ml, 10:1
– Temperature: injection port, column, detector
– Detection: e.g. flame ionisation detector (FID)
Test and standard solutions
System suitability testing (SST) and criteria: precision and
resolution, RSD (n=6)
Calculation
The prequalification programme--Assessor's training
24 | May 2015 25-28
Thin-Layer Chromatography - TLC
Mobile phase
A guard column may be used for HPLC, meet the following criteria:
– NMT 15% of the length of the analytical column
– the inner diameter ≤ analytical column
– the packing material must be the same (e.g. C18)
– All SSTs must be met