15 / 696
Table: Method Performance requirements for Amino acids as per SMPR 2014.013
3.6 - 45.0
± 10 %
45.0 - 450
± 8 %
450 - 22500 ± 5 %
3.6 - 45.0
≤ 4 %
45.0 - 450
≤ 3 %
450 - 22500 ≤ 2 %
3.6 - 45.0
≤ 6 %
45.0 - 450
≤ 4 %
450 - 22500 ≤ 3 %
Method of Analysis
NIST SRM 1849a
Reference
values(mg/100g)
Result
a
(mg/100g)
Recovery
%
RSDr %
SMPR
Recovery
limits
b
, %
SMPR RSDr
limits
b
, %
Result (mg/100g) Recovery % RSD
R
%
SMPR
Recovery
limits
b
, %
SMPR RSD
R
limits
b
, %
315
319.7
101.5
2.3
92 - 108
≤ 3
316.1
100.3
2.4
92 - 108
≤ 4
37
34.5
94.4
2.4
90 - 110
≤ 4
37.7
102.9
4.9
90 - 110
≤ 6
720
683.4
94.9
1.3
95 - 105
≤ 2
706.3
98.1
2.2
95 - 105
≤ 3
400
369.4
92.4
1.6
92 - 108
≤ 3
378.9
94.7
3.7
92 - 108
≤ 4
241
230.1
95.5
3.2
92 - 108
≤ 3
234.0
97.1
2.9
92 - 108
≤ 4
1070
1099.5
102.8
2.2
95 - 105
≤ 2
1082.4
101.2
3.3
95 - 105
≤ 3
2590
2761.3
106.6
2.0
95 - 105
≤ 2
2725.6
105.2
2.5
95 - 105
≤ 3
640
619.1
96.7
0.9
95 - 105
≤ 2
613.5
95.9
1.7
95 - 105
≤ 3
455
445.5
97.9
1.5
95 - 105
≤ 2
442.0
97.1
2.7
95 - 105
≤ 3
1195
1173.8
98.2
0.7
95 - 105
≤ 2
1155.2
96.7
1.8
95 - 105
≤ 3
1010
1068.7
105.8
2.1
95 - 105
≤ 2
1064.6
105.4
4.0
95 - 105
≤ 3
510
476.6
93.4
2.6
95 - 105
≤ 2
471.3
92.4
3.8
95 - 105
≤ 3
NA
440.3
NA
1.6
NA
≤ 2
429.3
NA
1.9
NA
≤ 3
760
781.1
102.8
1.1
95 - 105
≤ 2
772.0
101.6
2.0
95 - 105
≤ 3
660
694.2
105.2
1.2
95 - 105
≤ 2
694.6
105.2
1.4
95 - 105
≤ 3
1261
1243.6
98.6
0.6
95 - 105
≤ 2
1219.8
96.7
2.1
95 - 105
≤ 3
580
561.3
96.8
2.3
95 - 105
≤ 2
552.2
95.2
3.5
95 - 105
≤ 3
128.6
138.4
107.6
1.6
92 - 108
≤ 3
131.8
102.5
4.2
92 - 108
≤ 4
NA
564.3
NA
1.7
NA
≤ 2
--
--
--
--
--
Alkaline hydrolysis followed
by UHPLC-FLD determination
184
173.3
96.8
--
92 - 108
≤ 3
--
--
--
92 - 108
≤ 4
a
Results reported are as is sample basis
b
SMPR limits are on 'reconstituted sample basis' and converted into 'as is sample basis' by multiplying with a factor 9
Prepared By: BKVR Prasad
Reviewed By: Meena Mariappan
Asst. Manager
General Manager - Chemical Testing
Product Service-COE
Product Service
TUV-SUD South Asia
TUV-SUD South Asia
Bangalore, India
Bangalore, India
3.6 to 22500 mg/100g
Limit of quantification (LOQ) on reconstituted product
≤ 0.4 mg/100g on reconstituted powder basis
3.6 mg/100g on as is basis
± 10 %
5.0 -50
± 8 %
Parameter
Minimum acceptable criteria
Analytical Range
0.4 to 2500 mg/100g
Acid Hydrolysis followed by
UHPLC-DAD determination
L-Methionine
Performic acid oxidation
followed by acid hydrolysis
and UHPLC-DAD
determination
Recovery
0.4 - 5.0
AMINO ACIDS METHOD VERIFICATION AGAINST AOAC SMPR 2014.013
L-Threonine
L-Glutamic acid
Cysteine + Cystine
Amino acid
L-Aspartic acid
L-Glycine
L-Argenine
L-Serine
L-Taurine
L-Histidine
L-Tryptophan
L-Lysine
L-Proline
L-Tyrosine
L-Alanine
L-Phenyl Alanine
L-Leucine
L-Isoleucine
L-Valine
L-Methionine
Repeatability
NIST SRM 1849a Results
Reproducibility
50 - 2500
± 5 %
Repeatability (RSDr)
0.4 -50
≤ 4 %
5.0 - 50
≤ 3 %
50 - 2500
≤ 2 %
Reproducibility (RSD
R
)
0.4 - 5.0
≤ 6 %
5.0 - 50
≤ 4 %
50 - 2500
≤ 3 %
Amino-03 (February 2016)
FOR ERP USE ONLY
DO NOT DISTRIBUTE