KS H 1207-2012 Methods of analysis for sugars《糖类测试方法》.pdf

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1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS H 1207 KS H 1207:2012 2012 12 29 http:/www.kats.go.krKS H 1207:2012 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) : :2002 2 28 :2012 12 29 2012-0834 : : ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS H 1207:2012 i 1 1 2 .1 3 .1 3.1 .1 3.2 .2 3.3 4

2、3.4 .6 3.5 .6 KS H 1207:2012 .22 KS H 1207:2012 Methods of analysis for sugars 1 ( .) . 2 , , , 3 3.1 3.1.1 a) 1) 1.1) n-: (4: 1: 2) 1.2) n-: (6: 4: 3) 2) 2.1) n- 10 % 2 % . . 2.2) - : (4: 1: 1) - 3 %, 0.01 % . 2.3) 1 % 0.2 N . b) 1) (1 5 g) 50 % 20 50 mL . . 1 4 % . 2) 2 5 L 1.1) 1.2) . 3) 2.1) 2.2

3、) 100 105 5 10 . 110 120 10 15 . 2.1) 2.2) . 2.3) . Rf . KS H 1207:2012 2 1 - : , , , , 1 2 % . Rf Rf , 2 Rf . 2 Rf n- : : n- : : (6: 4: 3) (4: 1: 5) (4: 1: 2) D- D- D- D- D- D- D- L- D- D- D- D- 0.39 0.34 0.46 0.42 0.50 0.43 0.56 0.59 0.24 0.32 0.40 0.16 0.72 0.32 0.28 0.18 0.16 0.20 0.23 0.28 0.21

4、 0.31 0.37 0.09 0.11 0.14 0.12 0.33 0.13 0.12 0.30 0.28 0.35 0.33 0.36 0.36 0.46 0.17 0.19 0.23 0.42 0.28 3.2 3.2.1 a) 1) A 40 g 1 000 mL . 2) B 200 g 150 g 1 000 mL . KS H 1207:2012 3 3) C ( .) 50 g 200 mL 1 000 mL . 4) D 5 g 1 000 mL 0.250 0 g 100 mL 2 mL 60 70 a mL 1 mL Cu 0.223 8/a g . b) 0.2 1.

5、0 g ( . .) 200 mL 80 %(v/v) 100 mL 1 . 250 mL . 250 mL . 100 mL 2 3 mL ( .) 30 mL 15 . 5 mL 3 . 10 % 5 mL 3 100 mL . c) 20 mL( 0.05 0.45 % .) 200 mL A B 20 mL 3 . 50 mL . 3 4 . . C 20 mL 3 4 . 100 mL D . D (mL) 1 . 3.2.2 . a) 1) (Na2HPO4 12H2O) 71 g, 40 g 400 mL 1 N 100 mL (CuSO4 5H2O 10 g 100 mL) 8

6、0 mL . (Na2SO4 10HSO) 410 g 1 N (KIO33.567 g 100 mL) 25 mL 1 000 mL . 1 2 . 0.01 3 mg/5 mL , 1 mg/5 mL . 1 mg/5 mL 10 mL, 0.5 mg/5 mL 5 mL . 2) 2.5 % . 3) 0.005 N (Na2S2O3 5H2O) 25 26 g 10 % 2 mL 1 000 mL 0.1 N , KS H 1207:2012 4 20 . 4) 1 N 200 , 0.005 N 10.0 mL 2.5 % 1 mL 2 N 2 mL 5 0.005 N . b) 3

7、.2.1 b) . c) 5 mL (25 mm200 mm) 5 mL . ( ). ( 3 ). 2 mL 2 N 1.5 mL . 5 0.005 N 0.5 % 1 mL . 0.05 mL . . 5 mL (mg) ( mL ) ( mL ) ( 3 ) 3 ( ) 25 35 25 35 15 25 15 25 25 35 35 45 15 25 25 35 30 40 0.143 0.127 0.135 0.135 0.135 0.175 0.135 0.260 0.216 3.3 3.3.1 3.2.1 b) 0.5 1 % 100 mL 250 mL 0.1 N 30 mL

8、 30 . 0.1 N 30 mL 250 mL . 20 mL 3.2.1 0.95 . 3.2 0.95 . 3.3.2 (0.15 % ) 3.3.1 . 5.0 mL 3.2.2 0.95 KS H 1207:2012 5 . 0.95 . 3.3.3 a) b) 3.2.1 b) . D () . . Lb=100mL)100(g/ b : t L : (dm) 20 20 b 66.5 LL= 504.15.66100mL)100(g/ ( , 6 .) 2 dm(200 mm) (g/ 100 mL)0.752 . 100 mL a g x % 100 mL ax/100(g)

9、. 752.0100=xax2.75(%) = 3.3.4 a) 1) (aumina) (alum) . 2) A (CuSO4 5H2O) 34.64 g 500 mL . A 10 mL 350 mL 40 mL, 30 % 4 mL 50 % 6 mL 0.1N . 8.174354.6 fAF= F : A A : 0.1 N (mL) KS H 1207:2012 6 f : 0.1 N , 10.005 . 3) B 173 g 50 g 500 mL . 4) 0.1 g 100 mL . b) 26 g 100 mL 5 mL . . 50 mL 25 mL 20 % 10

10、mL 67 100 mL 10 mL 250 mL . A B 5 mL 10 mL 200 mL 15 mL 2 1 % 4 . 1 3 . 1 2 mL . 2 100 mL (A) . 0.95 . 0001110010250100250(%) =SfA f : A S : (g) 3.4 3.4.1 3.4.2 a) , , 100 mL 50 mL 100 mL . b) 5 g 50 mL 25 mL 50 mL . 0.45 m . 3.4.3 a) 300 mm, 4 mm, -Bondapak/Carbohydrate b) (RI) c) : (17: 83)( .) d)

11、 1.0 mL/ ( .) e) 3.5 3.5.1 KS H 1207:2012 7 a) b) 1) HPLC 2) 3) (99.5 %) 4) ( ) 5) 80 % 99.5 % 80: 20(v/v) . 6) 5 % 5 g 100 mL 50 mL ( ). c) 1- (GF2), (GF3), 1-F (GF4) 0.4 g 20 mL 10 mL . 1, 2, 3, 4 5 mL 10 mL , 5 % 1 mL . d) 1) 0.2 2 g 100 mL 20 mL ( ). 5 % 20 mL . (No. 5B) . 25 mL 50 mL . (No. 5B)

12、 (No. 5B) 100 mL . 2) 0.2 2 g ( ). ( ). (602) 2 4 . , 816 . 3.5.1 d) 1) . . e) 1) 1.1) -Bondapak CH. PNH2-10 (Biosil Amino 5S, Shodex RSpak DC-613, Nueleosil NH2, Lichrosorb NH2 ) 1.2) : (65: 35) ( . 65:35 70: 30 . .) 1.3) 1.0 mL/min( .) 1.4) (RI) 2) 10 L . 10 L KS H 1207:2012 8 (GF2 GF3 GF4) . 0001

13、100100)(%)( +=EDCBA A : GF2 (mg/mL) B : GF3 (mg/mL) C : GF4 (mg/mL) D : E : (g) 3.5.2 a) b) 1) 50 % 2) 3) (H ) (OH ) 4) (perlite) 5) HPLC 6) 6.1) glucose, fructose 6.2) maltose, isomaltose1), sucrose, kojibiose1), nigerose1) 6.3) maltotriose, pannose1), isomaltotriose1) 6.4) maltotetraose, isomaltot

14、etraose1) 6.5) maltopentaose, isomaltopentaose1) 6.6) maltohexaose, isomaltohexaose1) 6.7) maltoheptaose, isomaltoheptaose1) c) 1) 50 mg 50 mL , 100 mL . 2) 100 mg 1 mL . d) 1) 500 mg (0.5 5 g) 50 % ( ) 30 mL , . 0.5 g ( 1: 2 1.5 g) , 500 mL . 2) (0.5 5 g) , (pH 4 10 ) 8 16 . 3.5.2 d) 1) . 2 5 , , ,

15、 coupling sugar 1) KS H 1207:2012 9 . , , . e) 1) 1.1) 1.1.1) 8 mm200 mm MCI GEL CKO 4S 1.1.2) 8 mm50 mm MCI GEL CKO 8S 1.1.3) 65 1.1.4) 1.1.5) 0.4 mL/min( .) 1.1.6) (RI) 1.2) 1.2.1) 4.6 mm250 mm TSK GEL NH2-60 1.2.2) 35 1.2.3) : (63: 37)( .) 1.2.4) 0.8 mL/min( .) 1.2.5) (RI) 2) 2.1) 5, 10, 15, 20,

16、25 mL 50 mL ( 25, 50, 75, 100, 125 mg/50 mL .) 10 L . 2.2) . DP1( ): A DP2( ): B DP3( ): C DP4( ): D DP5( ): E DP6( ): F DP7( ): G 2.3) (%) . DP1 fructose A1 DP1 glucose A2 DP2 maltose B1 DP2 sucrose B2 DP2 isomaltose B3 DP2 nigerose B4 DP2 gojibiose B5 DP3 maltotriose C1 DP3 pannose C2 DP3 isomalto

17、triose C3 DP3 ( ) C4 DP4 maltotetraose D1 DP4 isomaltotetraose D2 DP5 maltopentaose E1 DP5 isomaltopentaose E2 DP6 F DP6 isomaltohexaose F2 KS H 1207:2012 10 DP7 maltoheptaose G1 DP7 isomaltoheptaose G2 DP8 H DP4 DP8 . DP1 Fructose mgmg1211aAAAA =+ DP1 Glucose mgmg2212aAAAA =+ DP2 Maltose mgmg154321

18、1bBBBBBBB =+ DP2 Sucrose mgmg2543212bBBBBBBB =+ DP2 Isomaltose mgmg3543213bBBBBBBB =+ * DP2 Negerose mgmg4543214bBBBBBBB =+ * DP2 Kojibiose mgmg5543215bBBBBBBB =+ * DP3 Maltotriose mgmg143211cCCCCCC =+ DP3 Pannose mgmg243212cCCCCCC =+ * DP3 Isomaltotriose mgmg343213cCCCCCC =+ * DP3 ( ) mgmg443214cCC

19、CCCC =+ * DP4 Maltotetraose mgmg1211dDDDD =+ DP4 Isomaltotetraose mgmg2212dDDDD =+ * DP5 Maltopentaose mgmg1211eEEEE =+ DP5 Isomaltopentaose mgmg2212eEEEE =+ * DP6 mgmg f = F KS H 1207:2012 11 DP6 Maltohexaose mgmg1211fFFFF =+ DP6 Isomaltohexaose mgmg2212fFFFF =+ * DP7 Maltoheptaose mgmg1211gGGGG =+ DP7 Isomaltoheptaose mgmg2212gGGGG =+ * DP8 mgmg hH = I mg L , * 100)(%) 2222432543+= ILgfedcccbbb

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