FENX I HUAXUE) Chinese Journal of Analytical Chem istry ) ; AS20500A U ltrasonic Cleaner p, p (No )

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1 33 FENX I HUAXUE) ( Chinese Journal of Analytical Chem istry , (,330047) 2 (,330047) %,,,, GC2ECD ( n = 5) 78. 6% % 86. 5% %, 3. 6% 8. 7% 4. 4% 10. 2% : mg/kg, mg/kg,,,, 1 80%,,,, [ 1 4 ],,, [ 5, 6 ], [ 7 ],, [ 8, 9 ],,,,,,,,, Agilent 6890N(Agilent), 63 N i2ecd ; DS21 ( ) ; DSY2 ( ) ; RE252A ( ) ; TDL252A( ) ; XK962A ( ) ; AS20500A U ltrasonic Cleaner p, p 2 p, p 2 o, p 2 p, p 2 (, 100 mg/l) ;(RDH) ; ;, ;(, h) ; Florisil(, h 1305 h) ;(, h) g 100 ml,,100 mg/l, 100 mg/l p, p 2 p, p 2 o, p 2 p, p ; (No )

2 5 : , m 530 mm mm () : 60 (2 m in) 15 /m in 270 ( 8 m in ) ; : 300 ; : 250 N2 : 3 ml /m in () ; (N 2 ) : 60 ml /m in 1. 0 ml; :, , mm, 1. 0 g 20 ml, 2 ml 30%,, 15 m in,2 ml 5%,, 2 ml,, 15 m in, 3600 r/m in5 m in, 10 ml,2 ml,, 2 ml cm, 1 g, 5 g 1 cm,,, 20 ml,,20%, m in 1 2 ml, 30 ml,, ml, 1. 0 L D 21701, D 21701, ; ( 1),, 1 Fig. 1 Chromatogram of pesticides standards 1. 2 ( 2benzenehexachloride) ; 2. 2 ( 2benzenehexachloride) ; 3. ( hep tachlor) ; 4. ( aldrin) ; 5. 2 ( 2benzenehexachloride) ; 6. 2 ( 2benzenehexachloride) ; 7. ( p, p 2dichlorodiphenyl dichloroethene) ; 8. ( dieldrin) ; 9. ethane) ; 10. p, p 2 ( p, p 2dichlorodiphenyl dichloroethane) ; 11. p, p 2 o, p 2 ( o, p 2dichlorodiphenyl trichloro2 p, p 2 ( p, p 2dichlorodiphenyl trichloroethane) ; 12. ( bifenthrin) ; 13. ( fenp ropathrin) ; 14. ( 2cyhalo2 thrin) ; 15. ( cypermethrin) ; 16. ( fenvalerate) ; 17. ( s2fenvalerate) ; 18. ( 2fluvalinate) ; 19. ( deltamethrin) g,0. 5 ml, 100 ml2 6 8 h,, 10 ml, 2 ml, 5 ml, 1 ml , 80. 8% %,, g,0. 1 ml, 2 ml2

3 m in,2 ml 5% NaCl 2 ml, 5 m in,,2 ml, 2 ml, 1 ml, 1 ml , 87. 6% %,,,, g,0. 1 ml, 2 ml 30%,, 15 m in 2 ml 5% NaCl 2 ml,, 15 m in, 3600 r/m in5m in,,2 ml, 2 ml, 1 ml, 1 ml , 78. 6% %,,,,, 3. 3 ( 0. 5 mg/l mg/l ) mg/l ,,, mg/l, mg/l (1) 1 19 Table 1 The linear equation and correlation coefficient Pesticides L inear equation Correlation coefficient 2 2Benzenehexachloride ( 2BHC) y = x Benzenehexachloride ( 2BHC) y = x Hep tachlor y = x A ldrin y = x Benzenehexachloride ( 2BHC) y = x Benzenehexachloride ( 2BHC) y = x p, p 2 p, p 2D ichlorodiphenyl dichloroethene ( p, p 2DDE) y = x D ieldrin y = x o, p 2 o, p 2D ichlorodiphenyl trichloroethane ( o, p 2DDT) y = x p, p 2 p, p 2D ichlorodiphenyl dichloroethane ( p, p 2DDD) y = x p, p 2 o, p 2D ichlorodiphenyl trichloroethane ( p, p 2DDT) y = x B ifenthrin y = x Fenp ropathrin y = x Cyhalothrin y = x Cypermethrin y = x Fenvalerate y = x s2fenvalerate y = x Fluvalinate y = x Deltamethrin y = x ml 100 L,,25, (2),, mg/kg 89. 1% % ;0101 mg/kg 67. 3% 87. 5% mg/kg, mg/kg, mm,,,, 3,,, 20, 4

4 5 : 617, 4 2( n = 5) Table 2 Results of recovery tests ( n = 5) Pestcides mg/kg mg/kg mg/ kg organochlorines mg/kg pyrethroids ( % ) Recovery RSD ( % ) 0. 5 mg/kg+ 1. 0mg/kg 0. 5 mg/kg organochlorines mg/ kg pyrethroids ( % ) Recovery 2 2BHC BHC Hep tachlor A ldrin BHC BHC p, p 2 p, p 2DDE D ieldrin o, p 2 o, p 2DDT p, p 2 p, p 2DDD p, p 2 p, p2ddt B ifenthrin Fenp ropathrin Cyhalothrin Cypermethrin Fenvalerate s2fenvalerate Fluvalinate Deltamethrin (mg/kg) Table 3 Determ ination results of pesticide residues in Chinese herbal medicines (mg/kg) Pesticides F ructus gardeniae Determ ination results(mg/kg) Rhizom a atractylodi2 sm acrocephalae Salvia m iltiorrhizabunge 2 2BHC BHC RSD ( % ) Radix Isatidis Hep tachlor A ldrin BHC BHC p, p 2- p, p 2DDE D ieldrin o, p 2 o, p 2DDT p, p 2 p, p 2DDD p, p 2 p, p 2DDT B ifenthrin Fenp ropathrin Cyhalothrin Cypermethrin Fenvalerate s - Fenvalerate Fluvalinate Deltamethrin ( note) : - ( not detected or lower than lim its of detection) References 1 Cong Xiaodong( ), L i Ying( ), FangW ei( ), Chen B ilian ( ), Yu J ianp ing( ). Journal of

5 China Pharm aceutical U niversity (), 1999, 30 (2) : Zhang Shum ing( ), Guo Huaizhong( ), Chen J ianm in ( ). China Journal of ChineseM ateria M edical( ), 2000, 25 (7) : Zhang Shum ing( ), Guo Huaizhong ( ), Chen J ianm in ( ). A cta Pharm aceutica S inica ( ), 2000, 35 (8) : Gao Tianbing( ), Zhang Shum ing ( ), Tian J ingai ( ). Journal of Instrum ental A nalysis ( ), 1999, 18 (2) : L i Yongjun ( ), Huang Zhiqiang( ), Dai Hua ( ), Zhang Ying( ). Chinese J. A nal. Chem. ( ), 2002, 30 (7) : Zhang Ying( ), Huang Zhiqiang( ), L i Yongjun ( ), Xiong Fang( ). Chinese J. A nal. Chem. ( ), 2002, 30 (3) : L in W eixuan ( ). The Com pilcation of R esidue L im its S tandards for Pesticides and V eterinary D rugs in Foodstuffs in the W orld ( ). Dalian () : Dalian Maritime University Press( ), 2003: Editorial Group of State Adm inistration Commodity Inspection (). The Com prehensive Com pilation of A nalysis for Foodstuffs, Vol. 1 ( ( ) ). Beijing () : H igher Education Press ( ), 1997: Fan Defang( ). The A nalysis and D eterm ination of Pesticide Residues( ). Shanghai() : Shanghai Science Press( ), 1982 D eterm ina tion of O rganochlor ine and Pyrethro id Pestic ide Residues in Ch inese Herba lm ed ic ines W an Yiqun 3 1, 2, Yan A ip ing 2, Xie M ingyong 1 ( The Key Laboratory of Food Science of M inistry of Education 1, Center of A nalysis and Testing 2, N anchang U niversity, N anchang ) Abstract A new method for multiresidue analysis of eleven organochlorines and eight pyrethroids in Chinese herbal medicines in J iangxi p rovince is p roposed. Pesticide residues were extracted from Chinese herbal medi2 cine samp les with n2hexane followed by acetone2acetonitrile (3 7, V /V ). Extracts were cleane2up by alum ina neutral2florisil column. Analytical screening was determ ined by gas chromatography using pesticide residue cap illary column equipped w ith electron2cap ture detector. The recoveries obtained from Chinese herbal medicine samp les ( n = 5) at two concentration levels were in the ranges of 78. 6% % and 86. 5% 11410%, with relative standard deviations of 3. 6% 8. 7% and 4. 4% 10. 2%, respectively. L im its of detection were mg/ kg for organochlorines and mg/ kg for pyrethroids. A satisfactory result was obtained in the determ ination of organochlorines and pyrethroids in Chinese herbal medicines of J iangxi p rovince. Keywords O rganochlorine pesticide, pyrethroid pesticide, residue analysis, Chinese herbal medicine (Received 15 January 2004; accep ted 29 November 2004)