ENV IRONM ENTAL CHEM ISTRY

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1 ENV IRONM ENTAL CHEM ISTRY Vol. 29, No. 3 May , 2 1, 2 1, 233 1, 2 1, 2 1, 2 1, 2 (1,, ; 2,, ) 2 6. ( ) 5m l ( 2g 011g 011gNa 2 EDTA ) 25m in, 2, C 18. (0101mol l - 1, ph215) = (V V ), 270nm % 9819%, g kg - 1., 6, mg kg - 1 ( ).,,. ( SA s). [ 1 ]. [ 2, 3 ], ( ), [ 4 9 ]., [ 10, 11 ], [ 12 ],.,, [ 13 ],., (CAC) (MRL) [ 13 ]. ( ), [ ]..,, / (HPLC /MS).,, Shimadzu, Shimadzu LC2LC220AT, Shimadzu SIL220A, Shimadzu SPD220AV,, LC Solution ; ; KDC2 160HR ; SHZ282 ; KQ2250E ; 24 ; Oasis C 18 ( 3m l/500mg, Supelco) ; HLB ( 3m l/500mg, Supelco) ; PHS23C ph ;. ( ST) ( SPD ) ( SM1) ( SM2) 252 ( SMT) ( SMZ), D r. Ehrenstorfer, > 9810% ( , ) ; ( ) ; (2005B , 2006B ) ; ( ) ; (2009B ). 3 3, Tel: , E2mail: tchmo@ jnu1edu1cn

2 Na 2 EDTA2Mcllvaine : 1219g, 2715g, 3712g, 1L. A: Na 2 EDTA2Mcllvaine 2 ( 1 4, V V ) [ 17 ] ; B 2 (50 50, V V, 25mmol l 21, 10 mmol l - 1 Na 2 EDTA 10 mmol l - 1, ph = 8110) ; C: ( Na 2 EDTA ) g 50m l,,, 10 (8000 r m in - 1 ) 15m in,, 2,. 10m l 2 2,, [ 12 ]., 1m l. 20m l Na 2 EDTA2Mcllvaine, C 18. 6m l, 6m l,, m in - 1, 6m l, 3m l, 40 m in , 1m l 2 (1 1, V V ), 0122 m,. : Symmetry C 18 (416mm 250mm, : 110m l m in - 1 ; : 20 l; : 25 ; : 270nm m ) ; : ( 0101mol l - 1 ) ;.,. 5m l ( ) (1g), 6 ( 5 g g - 1, ) 1 ( C 18 )., A B 6, SM2 5, (9192% 39177% ) ; C1 ST SPD SM2, SM1 SMT SMZ ; C2 ST, SM1 ; C3 SPD ; C4 6 60%, 98191%,,, 1. C4 ( + 2g Na 2 SO 4 1 ( % ) + 011g CH 3 COONa + 011g Na 2 EDTA). Table 1 Recovery of sulfonam ide antibiotics in vegetable by different extraction ( % ) ST SPD SM1 SM2 SMT SMZ A B C1 ( + 2g Na 2 SO 4 ) C2 ( + 2g Na 2 SO g Na 2 EDTA) C3 ( + 2g Na 2 SO g CH 3 COONa) C4 ( + 2g Na 2 SO g CH 3 COONa g Na 2 EDTA) C4 6 11ST, 21SPD, 31SM1, 41SM2, 51SMT, 61SMZ F ig11 Chromatogram s of six sulfonam ide antibiotics

3 3 : C4 (C 18 HLB ( ) ), ; HLB (2cm ) ST (20197% 31152% ) ; C 18 (4cm) 6, 58108% 98191% 63115% 90140%, (60133% % )., [ 18, 19 ]. (4cm), C 18 [ 18, 19 ]., C ( % ) Table 2 Recovery rate of 6 sulfonam ide antibiotics treated by different columns ( % ) ST SPD SM1 SM2 SMT SMZ C HLB (4cm) (2cm) (4cm) C4 1100g 6 ( 2),, 5m l 6., 1g 5m l,, 3. SM1 ; ST SPD, 25m in 30m in ; SM2 SMT 25m in ; SMZ 20m in 25m in. 25m in. 2 3 F ig12 Effect of extraction volume on recovery rate of sulfonam ide antibiotics F ig13 Effect of ultrasonic time on recovery rate of sulfonam ide antibiotics 214, ph, ( ). (0101mol l - 1 ), ph,. ph 215, ( 4). (0101mol l - 1 ), 6, ; (0101mol l - 1 ),,,., ( 0101mol l - 1, ph = 215) = (V V ), 6,,

4 516 29, ST, 21SPD, 31SM1, 41SM2, 51SMT, 61SMZ F ig14 Effect of mobile phase on separation of sulfonam ide antibiotics g m l g m l g m l g m l g m l g m l g m l - 1., 6 ( y) ( x) ( 3), R > ( ) g, g kg Table 3 Regression analysis of calibration curves and quantification lim its for sulfonam ide antibiotics (R ) / g kg - 1 ST SPD SM1 SM2 SMT SMZ y = x y = x y = x y = x y = x y = x , 12h,, C 18,, % 98191%, RSD ( 4),, ( % ) ( % ) ( n = 4) Table 4 Recovery rate ( % ) and RSD% of 6 sulfonam ide antibiotics in vegetable ( n = 4) / g g - 1 ST SPD SM1 SM2 SMT SMZ (6199) (4132) (3120) (4186) (6139) (3139) (4108) (3146) (5129) (8111) (3158) (8163) (8142) (2144) (4177) (4168) (6167) (5196) 216 ( ),, 5 ( ).,, mg kg - 1 ( )

5 3 : ,. 5 6 (mg kg - 1, ) Table 5 Analytical results of sulfonam ide antibiotics in different vegetables(mg kg - 1, F W ) ST SPD SM1 SM2 SMT SMZ ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND ND : ND. 3 6, 50184% 98191%, g kg - 1.,., mg kg - 1 ( ).,,. [ 1 ] M ichael P S, Kai B, Persistence of Antibiotics Such as Macrolides, Tiamulin and Salinomycin in Soil [ J ] 1Environm ental Pollution, 2006, [ 2 ] Bevill R F, Factors Influencing the Occurrence of D rug Residues in Animal Tissues after the U se of Antim icrobial Agents in Animal Feeds [ J ] 1 JAVMA, 1984, 185 (10) [ 3 ] Lunestad B T, Samuelsen O B, Fjelde S et al1, Photostability of Eight Antibacterial Agents in Seawater [ J ] 1 Aquaculture, 1995, [ 4 ] Sarmah A K, MeyerM T, Boxall A B A, A Global Perspective on the U se, Sales Exposure Pathways, Occurrence, Fate and Effects of Veterinary Antibiotics in the Environment [ J ] 1 Chem osphere, 2006, [ 5 ] N icole Kemper, Veterinary Antibiotics in the Aquatic and Terrestrial Environment [ J ] 1 Ecological Indicators, 2008, [ 6 ] Xu W H, Zhang G, L i X D et al1, Occurrence and Elim ination of Antibiotics at Four Sewage Treatment Plants in the Pearl R iver Delta ( PRD), South China [ J ] 1W ater Research, 2007, [ 7 ],,, 2 3 [ J ] 1, 2007, [ 8 ],,, 2 / [ J ] 1, 2006, 25 ( 2) [ 9 ],,, [M ] 1 :, 2004, 393 [ 10 ] Ben W W, Q iang Z M, Adam s C et al1, Simultaneous Determ ination of Sulfonam ides, Tetracyclines and Tiamulin in Swine W astewater by Solid2Phase Extraction and L iquid Chromatography2Mass Spectrometry [ J ] 1 Journal of Chrom atography A, 2008, [ 11 ] Jacobsen A M, Bent H S, Ingerslev F et al1, Simultaneous Extraction of Tetracycline, Macrolide and Sulfonam ide Antibiotics from Agricultural Soils U sing Pressurised L iquid Extraction, Followed by Solid2Phase Extraction and L iquid Chromatography Tandem Mass Spectrometry [ J ] 1 Journal of Chrom atography A, 2004, [ 12 ] K mmerer K, Antibiotics in the Aquatic Environment2A Review2Part I [ J ] 1Chem osphere, (4) [ 13 ],,, [M ] 1 :, 2007: [ 14 ] Maia P P, Rath S, Reyes F G, Determ ination of Oxytetracycline in Tomatoes by HPLC U sing Fluorescence Detection [ J ] 1Food Chem istry, 2008, [ 15 ] M igliore L, B rambilla G, Cozzolino S et al1, Effect on Plants of Sulphadimethoxine U sed in Intensive Farm ing ( Panicum m iliaceum, P isum Sativum and Zea M ays) [ J ] 1A griculture Ecosystem s & Environm ent, 1995, [ 16 ] M igliore L, Salvatore C, Maurizio F, Phytotoxicity to and Up take of Enrofloxacin in Crop Plants [ J ] 1 Chem osphere, 2003,

6 [ 17 ],,, [ J ] 1, 2008, 36 (7) [ 18 ], [M ] 1 :, 2008, [ 19 ],, ( 2 ) [M ] 1 :, 2006, 2 4 D ETERM INAT IO N O F S IX SUL FO NAM ID E ANT IB IO T ICS IN VEGETABL ES BY SOL ID PHASE EXTRACT IO N AND H IGH PERFO RM ANCE L IQU ID CHROM ATO GRAPHY BAO Yan2ping 1, 2 L I Yan2w en 1, 2 MO Ce2hui 1, 2 YAO Yuan 1, 2 TA I Yi2ping 1, 2 WU X iao2lian 1, 2 ZHAN G Yan 1, 2 (1 Department of Environmental Engineering, Jinan University, Guangzhou, , China; 2 Key Labratoty of W ater/soil Toxic Pollutants Control and B ioremediation, Department of Education of Guangdong Province, Guangzhou, , China) ABSTRACT In this paper a new analytical methodology for the simultaneous analysis of six sulfonam ides in vegetables using high performance liquid chromatography ( HPLC) w ith solid2phase extraction was p resented1 Vegetable samp les were extracted by acetonitrile ( adding 2g anhydrous sodium sulfate, 011g sodium acetate and 011g disodium ethylenediam ine tetraacetate), defatted by a double liquid liquid partition w ith n2hexane, dried in a rotary evaporator, then purified and enriched by the C 18 solid phase extraction column1 U sing acetonitrile and 0101mol l - 1 phosphoric acid (ph = 215 with triethylam ine) as the mobile phase, 270nm as detection wave2 length, the recoveries rate were 50184% 98191% and the detection lim its for six sulfonam ides in vegetables were obtained from to g kg The method was successfully app lied to determ ine six sulfona2 m ides in various vegetable samp les with the total contents of mg kg - 1 ( FW ) 1 Keywords: sulfonam ide antibiotics, high performance liquid chromatography, vegetable1