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Table 2016.16A. SMPR 2016.003 and First Action
Official Method
SM
2016.16 results
Type of
study
Parameter
Requirement
LC method results
Single-
laboratory
validation
LOQ, %
≤0.1 (w/w)
CUR
a
0.16
DMC
b
0.03
BDMC
c
0.03
Recovery, %
95-110
CUR
100.9
DMC
99.8
BDMC
99.3
Analytical range,
%
≤0.1-50
(w/w)
>50 (w/w)
≤0.1-50
(w/w)
>50 (w/w)
Repeatability
(RSD
r
), %
≤5
≤3
CUR
0.4-4.0
0.3-3.2
DMC
0.9-4.1
ND
d
BDMC
1.2-5.5
ND
Multi-
laboratory
validation
Reproducibility
(RSD
R
), %
≤8
≤5
CUR
ND
ND
DMC
ND
ND
BDMC
ND
ND
a
CUR = Curcumin.
b
DMC = Demethoxycurcumin.
c
BDMC = Bisdemethoxycurcumin.
d
ND = Not determined.
Table 2016.16B. Approximate concentrations of curcuminoids in mixed calibration standards
Curcuminoid
Approximate concentration, μg/mL
Std 1
Std 2
Std 3
Std 4
Std 5
Std 6
Std 7
Curcumin (CUR)
300
225
150
100
50
10
5
Demethoxycurcumin
(DMC)
100
80
60
25
10
2.5
1
Bisdemethoxycurcumin
(BDMC)
120
75
40
25
10
2.5
1
Table 2016.16C. Preparation of mixed calibration standards
Solution
Volume, μL
Std 1
Std 2
Std 3
Std 4
Std 5
Std 6
Std 7
C-1000
300
225
150
100
50
DMC-1000
100
80
60
25
10
BDMC-1000
120
75
40
25
10
Std 4
100
Std 5
100
Methanol
480
620
750
850
930
900
900
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