AOACSPDSMethods-2017Awardsv2

27

Table 2016.16A. SMPR 2016.003 and First Action Official Method SM 2016.16 results

Type of study

Parameter

Requirement

LC method results

CUR a DMC b

0.16 0.03 0.03

LOQ, %

≤0.1 (w/w)

BDMC c

CUR DMC

100.9

Recovery, %

95-110

99.8 99.3

Single- laboratory validation

BDMC

Analytical range, %

≤0.1-50 (w/w)

≤0.1-50 (w/w) 0.4-4.0 0.9-4.1 1.2-5.5

>50 (w/w)

>50 (w/w)

CUR DMC

0.3-3.2

Repeatability (RSD r ), %

ND d

≤5

≤3

BDMC

ND ND ND ND

CUR DMC

ND ND ND

Multi- laboratory validation

Reproducibility (RSD R ), %

≤8

≤5

BDMC

a CUR = Curcumin. b DMC = Demethoxycurcumin. c BDMC = Bisdemethoxycurcumin. d ND = Not determined.

Table 2016.16B. Approximate concentrations of curcuminoids in mixed calibration standards

Approximate concentration, μg/mL

Curcuminoid

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) Bisdemethoxycurcumin (BDMC)

100

80

60

25

10

2.5

1

120

75

40

25

10

2.5

1

Table 2016.16C. Preparation of mixed calibration standards

Volume, μL

Solution

Std 1

Std 2

Std 3

Std 4

Std 5

Std 6

Std 7

C-1000

300 100 120

225

150

100

50 10 10

DMC-1000 BDMC-1000

80 75

60 40

25 25

Std 4 Std 5

100

100 900

Methanol

480

620

750

850

930

900