KS H ISO 9233-2006 Cheese and cheese rind-Determination of natamycin content-Method by molecular absorption spectrometry and by high-performance liquid chromatography《干酪和干酪外皮 游酶素含量.pdf

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1、KSKSKSKS SKSKSKS KSKSKS SKSKS KSKS SKS KS 2006 11 29 http:/www.kats.go.krKS H ISO 9233 ( ) KS H ISO 9233： 2006 (2011 )H ISO 9233： 2006 : ( ) ( ) ( ) ( ) : (http:/www.standard.go.kr) ： ： 2001 12 31 ： 2006 11 29 ： 2011 12 29 2011-0652 ： ： ( 02-509-7273) (http:/www.kats.go.kr). 10 5 , . ICS 77.060 KS (

2、 ) H ISO 9233：2006(2011 ) Cheese and cheese rind Determination of natamycin content Method by molecular absorption spectrometry and by high-performance liquid chromatography 1991 1 ISO 9233 Cheese and cheese rind Determination of natamycin content Method by molecular absorption spectrometry and by h

3、igh-performance liquid chromatography . ISO 9233 ISO/TC 34 (SC 5), (IDF) (AOAC) , . A . 1. (natamycin) . 0.5 mg/kg . 1 mg/dm2(1) . . (1) EEC . 2. . . KS H ISO 707 3. . 3.1 . mg/kg , mg/dm2 . 3.2 5 mm . 4. . 15 20 . (HPLC) ( ) . 5. . . 5.1 5.2 1： 2(V/V) . 5.3 5 mg/L 50 mg 100 mL (5.1) . H ISO 9233： 2

4、006 2 5.0 mL 50 mL (5.2) 50.0 mL . 1 mL 5 g . 9.3.1.2 . . 5.4 6. . 6.1 (slicer) 3 cm 5 mm ( 1 ). 1 5 mm 6.2 (fine-slicer) 1 mm ( 2 ). 2 1 mm 6.3 6.4 . 6.5 (shaking machine) 6.6 100 200 mL . 6.7 10 mL 6.8 0.20 m 0.45 m . 6.9 (2) 15 cm . (2) S S, No. 595 1/2 . ISO . 6.10 7 cm . 6.11 15 20 . 6.12 C18 (

5、3) . (3) Sep-pack C18 Waters No. 51910 . 5 mm H ISO 9233： 2006 3 ISO . 6.13 1 cm 300340 nm . 6.14 303 nm UV . 6.15 4.6 mm, 150 mm 5 m C8 (4) (4) Lichrosorb RP 8 . ISO . 6.16 (guard column) 2.1 mm, 100 mm 3040 m C8 (5) (5) Lichrosorb RP 8 . ISO . 7. KS H ISO 707 . . 8. 8.1 3 cm . (6.1) 5 mm . (2040 c

6、m2) cm2 , g . . . , . 8.2 8.1 , (6.2) 1 mm . 0.5 cm2 . . , . 9. 9.1 200 mL (6.6) (8.1) 10 g 10 mg . 100 mL (6.6) (8.2) 5 g 10 mg . 9.2 (5.1) 100 mL , (5.1) 50 mL . (6.5) (6.5) 90 . 50 mL , 25 mL (6.11) 60 . (6.9) 5 mL . . (6.7) 0.45 m 0.20 m H ISO 9233： 2006 4 (6.8) . 3 mL , 1 20 L 5 10 25 mL 50 mL

7、(9.3.3). 9.3.1, 9.3.2 9.3.3 . 9.3 9.3.1 (Spectrometric measurement) 9.3.1.1 (Natamycin standard solution) 300340 nm (5.3) . 317 nm , 311 nm 329 nm . (5.2) . 3 . . 317 nm 311 nm . . 3 9.3.1.2 300340 nm . 317 nm , 311 nm , 329 nm . . , 9.3.3 . 4 . . 4 . , mm H ISO 9233： 2006 5 A , 61 mg/kg B , 15 mg/k

8、g C , 1.7 mg/kg D , 0.3 mg/kg E , C 5 F , D 10 4 9.3.2 9.3.2.1 (6.14, 6.15, 6.16) . ： / / , 60 40 5(V/V/V) ： 1 mL/min ： 303 nm, 0.005 , ： 10 mV ( ) theoretical(typical) plate count： 1 500 , mm H ISO 9233： 2006 6 (6.15) . (5.4) 303 nm . (9.3.2.2) . 9.3.2.2 50 mL (5.3) 1m L, 2 mL, 4 mL, 6 mL 8 mL (5.2

9、). 0.1 g/mL, 0.2 g/mL, 0.4 g/mL, 0.6 g/mL 0.8 g/mL . 20 L . g/mL , . 5 . . . 5 0.5 g/mL 9.3.2.3 20 L . . 9.3.3 . 6 . 0.001 H ISO 9233： 2006 7 A , 61 mg/kg B , 15 mg/kg C , 1.7 mg/kg D , 0.3 mg/kg E , C 5 F , D 10 6 9.3.3 9.3.3.1 5 10 . 9.3.1.2 9.3.2.3 . (9.2) 25 mL 50 mL( 5 10 ) 50 mL 100 mL . (6.7)

10、 35 mL C18(3) (6.12) 10 mL . (6.7) 25 mL/min 10 mL (5.1) 3 mL . 9.3.3.2 (9.3.3.1) 1.5 mL . (6.7) 0.45 m (6.8) 0.20 m (cell) 9.3.1.2 . 9.3.3.3 (5.1) 5 mL (9.3.3.1) 9.3.2.3 . 10. 10.1 WS (1) . Ws =NNtscAmAV (1) Ws： (mg/kg) cN： (g/mL) 0.001 H ISO 9233： 2006 8 AN： 317 nm As： 317 nm mt： (9.1) (g) V： (9.2

11、) (mL) AN 329 nm 311 nm ( 3 ) UV (2) . N329N2N1N)(31)(32)( AAAA = (2) (A1)N： 317 nm (A2)N： 311 nm (A329)N： 329 nm As 329 nm 311 nm ( 7 ) UV (3) . s329s2s1s)(31)(32)( AAAA = (3) (A1)s： 317 nm (A2)s： 311 nm (A329)s： 329 nm ws . 7 UV (4) ws ws (mg/dm2) . ws = wsAmr (4) ws： (mg/kg) A： (8.1) (dm2) mr： (8

12、.1) (kg) 9.3.3 ws ws . 5 ( )： 5.6 10 ( )： 11.1 H ISO 9233： 2006 9 10.2 (9.3.2.2) . ws(mg/kg) (5) . ws=tmmcV (5) cm： (g/mL) mt： (9.1) (g) V： (9.2) (mL) ws . , (4) ws ws (mg/dm2) . 9.3.3 ws ws . 5 ( )： 5 10 ( )： 10 11. 95 % ISO 5725(6) . (6) ISO 5725： 1986 pricision of test methods Determination of re

13、peatability and reproducibility for a standard test method by inter-laboratory tests 11.1 mg/dm2 1.3 g/cm3 5 mm mg/kg . 2 1 . 60 mg/kg(4 mg/dm2) 16 % HPLC 26 % 15 mg/kg(1 mg/dm2)60 mg/kg(4 mg/dm2) 17 % HPLC 20 % 10 15 mg/kg 45 % HPLC 65 % 10 0.31 mg/kg 120 % HPLC 80 % 11.2 mg/dm2 1.3 g/cm3 5 mm mg/k

14、g . 2 1 . H ISO 9233： 2006 10 60 mg/kg(4 mg/dm2) 35 % HPLC 60 % 15 mg/kg(1 mg/dm2)60 mg/kg(4 mg/dm2) 35 % HPLC 70 % 10 15 mg/kg 100 % HPLC 105 % 10 0.31 mg/kg 170 % HPLC 110 % 1 HPLC mg/dm2 mg/kg CVr % CVR % CVr % CVR % 4 1 60 15 5.9 6.2 12.2 11.9 9.3 7.1 20.6 25.7 0.08 0.02 1.3 0.3 16.5 42.5 35 60

15、23.4 29 37 39 10 CV = (coefficient of variation) rrel= 2.83CVr Rrel= 2.83CVR 8 1984 36 . 12. . . H ISO 9233： 2006 11 A() 1 DE RUIG, W.G., VAN OOSTROM, J.J. and LENNHEER, K. J. Ass. Off. Analytical Chem., 1987. vol. 70, pp. 944 948 2 DE RUIG, W.G. K. J. Ass. Off. Analytical Chem., 1987. vol. 70, pp.

16、949 954 ( ) 153787 1 92 3(13) (02)26240114 (02)2624 01489 http:/ KSKSKSSKSKS KSKS SKS KSKS SKSKS KSKSKSKS H ISO 9233： 2006 Cheese and cheese rindDetermination of natamycin contentMethod by molecular absorption spectrometry and by high performance liquid chromatography ICS 77.060 Korean Agency for Technology and Standards http:/www.kats.go.kr