Requirements for a Successful OQ/PQ
OQ/PQ Operating Instructions
M1393R0
Page 11 of 60
Linearity
(Section 4.7)
(c)
Injections of caffeine standards
covering the linear range of the
UV detector are injected and the
peak height is measured. The
regression coefficient of the
resulting calibration curve
indicates the linearity.
R
≥
99.50%
peak height
R
≥
99. 0%
peak height
Gradient
accuracy, step
gradient
(Section 4.10)
(c)
A step gradient is performed and
the UV trace recorded. The step
intensity indicates the gradient
accuracy.
Channel A: water
Channel B: water with 0.8 %
acetone (NAN configuration) or
0.3% acetone (CAP
configuration), respectively.
The range is
defined by the
0% and 100%
values.
A relative
deviation of 3%
is allowed for
each step (5%,
50%, 95%).
The range is
defined by the
0% and 100%
values.
A relative
deviation of 3%
is allowed for
each step (5%,
50%, 95%).
UltiMate
System
(Single and
Dual Gradient
Version)
Gradient
reproducibility
(Section 4.10)
(d)
A step gradient is programmed
and measured 3 times.
The reproducibility of the
proportioning is evaluated.
For each step,
the intensity of
the signal is
measured. The
maximum %RSD
allowed is 1%.
For each step,
the intensity of
the signal is
measured. The
maximum %RSD
allowed is 1%.
Reproducibility
of the injection
(Section 4.8)
(c) (d)
8 injections of a caffeine standard
are analyzed. The relative
standard deviation of the peak
height is calculated.
Peak height
RSD
≤
1.5%
Peak height
RSD
≤
1.5%
FAMOS
(Well Plate /
Carousel
Version)
Linearity of the
injection
(Section 4.9)
(d)
Partial loop injections of a
caffeine standard are performed
(from 0.05
µ
l to 0.5
µ
l). The
regression coefficient of the
resulting calibration curve
indicates the linearity.
R
≥
99.50%
(calculated via
peak area)
R
≥
99.0%
(calculated via
peak area)
Switchos fluid
path test
(Section 4.11)
The flow rate is measured for all
the channels.
The flow rate is
at least
0.15 mL/min.
The flow rate is
at least
0.15 mL/min.
Valve position
test
(Section 4.13)
The position and is switching of
the valves is checked.
LED indication
must correspond
to the open
channel on the
valve.
LED indication
must correspond
to the open
channel on the
valve.
Switchos
Switchos flow
rate and
pressure
stability
(Section 4.12)
(d)
The Switchos pump is
programmed to deliver a flow rate
of 30
µ
l/min. The output is
connected to one of the valves
with a restriction connected to
port 2. During this program the
valve is switched from position 1-
2 to 10-1. The backpressure must
be stable and reduce to zero
without restriction.
Flow rate must
be 30
±
3
µ
L/min
Pressure must be
18
±
5 bars
when restriction
is in line and 0
bars otherwise.
Flow rate must
be 30
±
3
µ
L/min
Pressure must be
18
±
5 bars
when restriction
is in line and 0
bars otherwise.
Notes:
a)
OQ limits with optimum measuring conditions, recommended PQ limits.
b)
The signal intensity should be
≥
5% of the reference signal for a 30 mm UV Booster
™
flow cell.
c)
Up to maximum signal height of CAP = 250 mAU or NAN = 30 mAU.
d)
All tests are performed by using the sequences provided with the IQ/OQ/PQ CD ROM.
