Chemistry Reference
In-Depth Information
tAble A.1
example robustness parameters and conditions
parameter
nominal value
condition 1
condition 2
Column temperature
30°C
27°C
33°C
Concentration acetonitrile in MP
40%
38%
42%
Mobile phase pH
3.8
3.6
4.0
Mobile phase flow rate
1.0 mL/min
0.90 mL/min
1.10 mL/min
A.4.7 m
ethod
r
obuStneSS
Method robustness is evaluated by measuring method performance toward typical or
normal variations in the method and detector operating parameters, for example, col-
umn temperature, mobile phase flow rate, and mobile phase composition, pH, buffer
concentration, etc. The effect (if any) of these variations can be determined by evalu-
ating the system suitability criteria. Example parameters and conditions that might
be tested are listed in the Table A.1. If any varied condition results in a failure to meet
requirements, it must be documented in the method and suitable controls put in place.
Any experimental design used to evaluate the different parameters should be
described.
A.4.8 d
egrAdAnt
lod
The LOD will often be established at 0.05% of the nominal concentration and evalu-
ated with at least one sample prepared at that concentration.
A.4.9 d
egrAdAnt
loQ
The LOQ will often be established at 0.1% of the nominal concentration, and evalu-
ated by measuring precision and accuracy of six separate samples prepared at the
target concentration.
A.4.10 S
olutIon
S
tAbIlIty
The stability of the stock reference standard and sample solutions is evaluated (dupli-
cate injections) at established intervals following storage at both room temperature
and refrigeration by assaying against freshly prepared standards prepared from a
freshly prepared stock solution.
A.5
dAtA evAluAtIon And reportIng
A.5.1 S
yStem
S
uItAbIlIty
This section should include any system suitability criteria to be measured, for exam-
ple, peak retention time and area (%RSD), resolution (peaks specified), the check
standard recovery, tailing, etc.
