1、 1 3 #1 2 3 1 1 100025 2 330002 3 10009 4 13 R P-H PLC SPE R P-H PLC - 13 0.06 5.0 m g /L 0.9 9 9 8 0.9 9 9 9 0.02 1 .0 g /g 71 .9 % 101 .9 % 2.3% 10.7% 2005- 10- 09 2005- 11 - 28 No .2003DIA 6 N003 1 40% 50% 1 0.1 m g /k g 0.05 m g /k g 0.3 m g /k g 0.02 m g /k g m e t r i b u z i n 0.1 m g /k g 2
2、3 4 13 H PLC H PLC 2 2 .1 H P 1100 A g i l e n t H P1100 C h e m s t a t i o n R e v .09 .01 Kr o m a s i l KR 100- 5C 18 KR 100- 5C 8 250 m m 4.6 m m i .d . 5 m Ek a C h e m i c a l s J2 s c i e n t i f i c a c c u p r e p GPC c l e a n u p s y s t e m s e r i e s p u m p DVW- 10v i r a b l e w a v
3、 e l e n g t h d e t e c t o r A c c u p r e p TM p r e p a r a t i v e LC s y s t e m Ex p r e s s TM c o l u m n 100% m e t h y l e n e c h l o r i d e 40g A c c u c h r o m e 13 9 7.0% Dr .Eh r e n s t o r f e r C o . Sc h a r l a u C h e m i e S.A . Mi l l i -Q 200 m g /L 2 . 2 10.00g 50m L 40m
4、L 2 m i n 30m i n 34 2006 6 FENXIH UA XUE C h i n e s e Jo u r n a l o f A n a l y t i c a l C h e m i s t r y 6 787 79 0 4000 r/min 5 min 32 120 r/min 1 mL N 2 10 mL J2 GPC 100% 5 mL/min 228 nm 14 min 24 min 50 mL 4 5 mL Al 2 O 3 -N SPE 6 mL/1000 mg 6 mL 1 mL/min N 2 1 mL - 8:2 V/ V 2.3 Kromasil KR
5、100-10C 18 250 mm 4.0 mm i. d. 5 m - 1 1. 0 mL/min 30 228 nm 10 L 1 Table 1 Gradient elution program Mobie phase Elution time min 0 2.0 11.0 12.0 16.0 27.0 28.0 35.0 H 2 O 80 65 60 57 57 40 35 25 Acetonitrile 20 35 40 43 43 60 65 75 3 3 .1 13 218 nm 222 nm 220 nm 220 nm 208 234 294 nm 224 nm 224 nm
6、218 nm 220 nm 224 nm 224 nm 218 nm 220 nm 228 nm 13 3.2 - - - 13 1 1 13 Fig.1 Chromatogram of the mixture of thirteen triazine herbicide standards 1.0 mg/kg 1. simetone 2. simazine 3 . cyanazine 4. atraton 5. metribuzin 6. simetryn 7. atrazine 8. prome- ton 9. terbumeton 10 ametryn 11. terbuthylazin
7、e 12. prometryn 13. dipropetryn 1 13 3.3 3. 3.1 - - 3.3.2 SPE GPC C 18 3 mL 500 mg 1.5 g + 2.0 g +0.5 g SCX 3 mL 500 mg Florisil 6 mL 1000 mg Al 2 O 3 3 mL500 mg 6 mL1000 mg C 18 + SCX Florisil Al 2 O 3 3 mL 500 mg 6 mL 1000 mg 13 2 8 8 7 34 GPC GPC GPC Al 2 O 3 6m L 10 0 0 m g GPC Al 2 O 3 Al 2 O 3
8、 GPC GPC Al 2 O 3 6 m L 10 0 0 m g 13 3 . 4 Y X m g /L 2 13 0 .0 6 5.0 m g /L 2 2 Ta b l e 2 Li n e a r e q u a t i o n s a n d c o r r e l a t i o n c o e f f i c i e n t s He r b i c i d e s Ra n g e o f l i n e a r i t y m g /L Li n e a r e q u a t i o n s Co r r e l a t i o n c o e f f i c i e n
9、 t s r He r b i c i d e s Ra n g e o f l i n e a r i t y m g /L Li n e a r e q u a t i o n s Co r r e l a t i o n c o e f f i c i e n t s r S i m e t o n 0 .0 6 5.0 Y = 73 . 0 4X -0 . 51 0 .9999 S i m a z i n e 0 .0 6 5.0 Y = 109. 26X +1. 11 0 .9999 Cy a n a z i n e 0 .0 6 5.0 Y = 71. 20 X +0 . 20 0
10、 .9999 At r a t o n 0 .0 6 5.0 Y = 71. 26X +0 . 25 0 .9999 Me t r i b u z i n 0 .0 6 5.0 Y = 3 0 . 70 X +0 . 58 0 .9997 S i m e t r y n 0 .0 6 5.0 Y = 97. 29X +0 . 3 6 0 .9998 At r a z i n e 0 .0 6 5.0 Y = 90 . 85X +0 . 83 0 .9998 Pr o m e t o n 0 .0 6 5.0 Y = 71. 24X -0 . 99 0 .9998 Te r b u m e t
11、o n 0 .0 6 5.0 Y = 64. 0 9X -0 . 99 0 .9999 Am e t r y n 0 .0 6 5.0 Y = 93 . 3 5X +0 . 28 0 .9998 Te r b u t h y l a z i n e 0 .0 6 5.0 Y = 90 . 72X +0 . 48 0 .9998 Pr o m e t r y n 0 .0 6 5.0 Y = 10 0 . 1X -0 . 60 0 .9999 S i p r o p e t r y n 0 .0 6 5.0 Y = 90 . 99X -0 . 11 0 .9999 Y p a a k a r e
12、 a X m g /L. 3 . 5 3 4 13 3 0 .0 2 1.0 g /g 13 71.9% 10 1.9% 2.3 % 10 .7% 0 .2 g /g HPLC 2 3 13 Ta b l e 3 Th e r e c o v e r i e s o f t h i r t e e n t r i a z i n e h e r b i c i d e s i n s o y b e a n s He r b i c i d e s Ad d e d m g /k g Re c o v e r y n = 10 % RS D % He r b i c i d e s Ad d
13、e d m g /k g Re c o v e r y n = 10 % RS D % He r b i c i d e s Ad d e d m g /k g Re c o v e r y n = 10 % RS D % S i m e t o n 0 .0 2 0 .0 5 0 .20 1.0 0 71.9 72.9 93 .0 87.9 2.3 9.8 5.3 5.3 S i m a z i n e 0 .0 2 0 .0 5 0 .20 1.0 0 95.2 86.1 94.2 92.8 7.7 8 .9 4.7 4.8 Cy a n a z i n e 0 .0 2 0 .0 5 0
14、 .20 1.0 0 76.4 76.2 88 .4 87.6 7.7 9.2 3 .1 4.7 At r a t o n 0 .0 2 0 .0 5 0 .20 1.0 0 88 .8 78 .9 95.4 91.6 4.4 4.2 6.2 3 .7 Me t r i b u z i n 0 .0 2 0 .0 5 0 .20 1.0 0 81.4 77.1 95.4 90 .9 8 .0 11.0 6.2 3 .8 S i m e t r y n 0 .0 2 0 .0 5 0 .20 1.0 0 79.8 80 .4 93 .5 93 .0 5.7 10 .7 3 .9 3 .3 At
15、r a z i n e 0 .0 2 0 .0 5 0 .20 1.0 0 79.9 78 .5 91.0 94.3 6.2 9.1 5.2 5.8 Pr o m e t o n 0 .0 2 0 .0 5 0 .20 1.0 0 10 1.9 85.5 90 .9 93 .4 3 .8 9.4 5.1 4.0 Te r b u m e t o n 0 .0 2 0 .0 5 0 .20 1.0 0 95.4 86.9 91.8 92.2 4.4 10 .6 5.3 4.2 Am e t r y n 0 .0 2 0 .0 5 0 .20 1.0 0 84.9 79.8 92.6 94.4 4
16、.8 10 .3 5.0 4.1 Te r b u t h y - l a z i n e 0 .0 2 0 .0 5 0 .20 1.0 0 89.7 79.3 91.7 93 .9 4.0 10 .7 4.8 4.2 Pr o m e t r y n 0 .0 2 0 .0 5 0 .20 1.0 0 81.0 77.0 95.8 94.8 6.9 9.8 5.3 4.1 Di p r o p e t r y n 0 .0 2 0 .0 5 0 .20 1.0 0 10 0 .3 85.4 95.2 95.5 3 .5 10 .6 5.3 4.2 13 9 8 7 6 13 20 g/kg
17、 2 0.2 g/g A B Fig.2 Chromatograms of soybean sample spiked with herbicide standards of 0.2 g/g A and blank sample B 1. simetone 2. simazine 3. cyanazine 4. atraton 5. metribuzin 6. simetryn 7. atrazine 8. prometon 9. terbumeton 10. ametryn 11. terbuthylazine 12. prometryn 13. dipropetryn References
18、 1 Yi Xianzhong Jiang Defeng . Journal of Laiyang Agriculture College 1999 16 1 25 27 2 Lin Weixuan . The Compilation of Residue Limits Standards for Pesticides and Veterinary Drugs in Foodstuffs in the World . Dalian Dalian Maritime University Press 2002 3 Balduini L Matoga M Seilles E. J. Chromato
19、gr. B 2003 794 389 395 4 Krutz L J Senseman S A Sciumbato A S. J. Chromatogr. A 2003 999 103 121 Simultaneous Determination of Thirteen Triazine Herbicides Residues in Soybeans by High Performance Liquid Chromatography Qi Yan #1 Zhan Chunrui 2 Zhang Xinzhong 3 Yang Qiang 1 1 Chinese Academy of Inspection and Quarantine Beijing 100025 2 Jiangxi Entry-Exit Inspection and Quarantine Bureau Nanchang 330002 3 Chinese Agriculture University
