2 (FDA) 1 1 A D E K 1 LC UV 15 HPLC 3.5 UHPLC Agilent 12 Infinity LC Agilent 12 Infinity (G1311B) Agilent 12 Infinity (G13E) Agilent 12 Infinity (G131

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1 1 Agilent 12 Infinity 1 Siji Joseph Agilent Technologies, Inc. Bangalore, India Agilent 12 Infinity (RP-HPLC) Agilent Poroshell EC-C1 Agilent 12 Infinity LC Agilent 12 Infinity (DAD) 2 D Agilent 12 Infinity LC (UHPLC)

2 2 (FDA) 1 1 A D E K 1 LC UV 15 HPLC 3.5 UHPLC Agilent 12 Infinity LC Agilent 12 Infinity (G1311B) Agilent 12 Infinity (G13E) Agilent 12 Infinity (G131C) Agilent 12 Infinity (G4212B) mm Max-Light Agilent 12 Infinity LC UHPLC Agilent 12 Infinity (G422 A) 1 µl Jet Weaver Agilent 12 Infinity (G422A) Agilent 12 Infinity (G131C) Agilent 12 Infinity (G4212A) 1 mm Max- Light : Agilent Poroshell 12 EC-C1 2.1 mm 5 mm 2. µm (5-2) Agilent Poroshell 12 EC-C1 3. x 15 mm 2. µm (35-32) : Agilent ChemStation B.4.2 HPLC Milli Q (Millipore Elix 1 Millipore ) Lab- Scan () (THF) Sigma ( ) Fluka ( ) (K3) (- ) ( A ) ( A ) -cis ( A ) K2 (D3) ( E ) K1 Aldrich ( ) 2

3 UHPLC 1 5 mg 25 ml K1 K2 D3 B 2. mg/ml (2, ppm) + 4. ºC 1 µl 2 ppm 1, µl B 2 ppm 5 pg/µl 1 ng/µl (1 ) 2 D 45 5 g D 2 1:1 1 ml D Agilent 12 Infinity LC : 45 ºC 45 ºC : 2 Hz Hz Agilent 12 Infinity LC : nm nm : mm 1 mm : 5 µl ( 5 ) : 5 ºC 5 ºC 1 µl ( 3 ) A : 5:5 : THF +.5 % 5:5 : THF +.5 % B : 5:25:5 : : THF +.35 % : 3 % B 3 5 % B 1 % B 15 1 % B % B : 5 1 5:25:5 : : THF +.35 % 5 % B. 5 % B 1. 1 % B % B % B :. ml/min. ml/min 1 Agilent 12 Infinity LC Agilent 12 Infinity LC 1. ml 2 µl B HPLC / 25 ng D 1 4 ºC 4 ºC D 5 µl B (RT) (SD) (RSD) LOD LOQ D 3

4 5 g 1 25 ng D / UHPLC LOD LOQ RT RSD UHPLC Agilent Poroshell 12 EC-C1 (3. mm x 15 mm 2. µm) nm ChemStation 12 4 DAD1A, Sig = 21 DAD1D, Sig = > > cm Agilent Poroshell 12 EC-C1 3 A Sl RT 1 K < A A cis A 3.55 K2 K D E < K1 K

5 (LOD) (LOQ) S/N 3 LOD S/N 1 LOQ LOD LOQ 3 ( D) LOD LOQ 2 LOQ LOQ LOD DAD1 C, Sig = 2 LEVEL 5 PG_LOQ DAD1 C, Sig = 2 LEVEL 25 PG_LOD DAD1 C, Sig = 2, BLANK ( D) LOD (25 pg) LOQ (5 pg) Sl LOD (ng) LOQ (ng) (ng) R 2 = y = x y =1.122 x y = x y = x y = x K y = x y = 1.24 x y =.413 x K y = x LOD LOQ 5

6 (RT) 5 ng (RT) (RSD) RSD.35 % RT RSD.4 % RT RSD 4 3 % 5 % 4 RT K2 K = 1.24*Amt 5.24 : [ng] ng () RSD RT RSD RSD RT RSD K2 K1 4 5 ng RT RSD

7 Sl () RT ( 3. %) ( 5. %) 1 (.) 2 %.2 ml/min. ml/min 2 (5 µl) 2 % 5.1 µl 3 ( ) 4. µl 1 % 4.5 (5.5 1) 5 ( 4 ) 5.5 ( ) 5 ( 4 ) 4 (ACN 5 %) 5 % % (:15:5) % (:25:5) 5 (45 ºC) 5 % 4.2 ºC ( nm) 42. ºC 3 nm ( nm) ( nm) 5 4 D D 3 25 ng/µl D D 4 % 2 % D DAD1 C Sig = 2 STD DAD1 C Sig = DAD1 C Sig = : : 12. :

8 D KOH D.3 µg/1 g 1 µg/. µg/1 g 12. µg/ Agilent 12 Infinity LC Agilent 12 Infinity LC cis. K2... K1 UHPLC UHPLC UHPLC 15 HPLC % ( ) ( ) ( ) A LOD LOQ UHPLC LOD LOQ 5 D 1 µ 1 ppm RT RSD RSD 1.25 % RT RSD.12 % Agilent 12 infinity HPLC 12 Infinity LC UHPLC Sl LOD (ng) LOQ (ng) RT RSD UHPLC (ng) R K K Agilent 12 Infinity LC UHPLC LOD LOQ =

9 54231 Agilent Poroshell 12 EC-C1 Agilent 12 Infinity LC 15 HPLC A D E K D % Agilent 12 Infinity LC 3 UHPLC Agilent 12 Infinity LC Agilent 12 Infinity LC = 3.221*Amt :. 2 4 [ng]..5 5 ng D ( ) 1 µl % RSD (1 ng ) RSD RT RSD K2 K1 1 ppm UHPLC RT RSD 1 µl

10 1. Analysis of water-soluble vitamins from multivitamin tablets for nutrition labeling, Agilent Application Note, publication number: 5-5EN, Leo M.L. Nollet, Food analysis by HPLC, Second edition revised and expanded, Chapter:, Page: Duncan Thorburn Burns, Klaus Danzer, and Alan Townshend, Use of the terms recovery and apparent recovery in analytical procedures, Pure Appl. Chem., Vol. 4, No. 11, pp , 22. 1

11 11

12 Agilent Technologies, Inc., 211 Published in Japan, September 1, JAJP

(DHA) 1 4 6 µg/ml 2,3 4 DHA AOAC 967.22 DHA C UVDHA 22 nm ph 244 265 nm 5 AOAC 994.11 UV UV HPLC Milli Q (Millipore Elix 1 ) Lab-Scan ( ) Fluka () o-

(DHA) 1 4 6 µg/ml 2,3 4 DHA AOAC 967.22 DHA C UVDHA 22 nm ph 244 265 nm 5 AOAC 994.11 UV UV HPLC Milli Q (Millipore Elix 1 ) Lab-Scan ( ) Fluka () o- Agilent Syed Salman Lateef Agilent Technologies, Inc. Bangalore, India 8 6 4 2 1.191 1.678 12.46 2.5 5 7.5 1 12.5 ( C) ( ) Agilent Poroshell EC-C18 Agilent 126 Infinity LC (LOD).2 µg/ml 3 9 % Agilent 129