HS - SPME - GC - MS. Abstract: Objective A rapid method was developed for multi2residues determination of organochlorine and pyrethroids

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1 HS SPME GC MS 289 HS SPME GC MS 1, , (11, ; 21, ; 31, ) :, 31 (23, 8 ), 6 10, gΠL,85 %110 %,3 %12 % : ;;,; ;,; Headspace Solid2Phase Microextraction Combined with Gas Chromatography Mass Spectrometry for Determination of Organochlorine and Pyrethroid Pesticides in Milk ZHU Jie, YANG Xin, FENGJin2fang, SHI Zhi2xiong, ZHAO Yun2feng, ZHOU Yan2ming, WU Yong2ning (College of Food Science, Shenyang Agriculture University, Liaoning Shenyang , China) Abstract: Objective A rapid method was developed for multi2residues determination of organochlorine and pyrethroids pesticides. Method Headspace solid2phase microextraction (HS2SPME) was used as sample pretreatment method for extraction and concentration. Gas chromatography with mass spectrometry detection ( GC2MSD) was used to analyze 31 pesticides (included 23 organochlorine pesticides and 8 pyrethroids) in milk. Two stable isotope compounds, 6 labeled hexachlorobenzene and 10 labeled mirex, were used as internal standards for the quantification. Results The method showed good recoveries (range from 85 % to 110 %) and repeatability ( RSD < 12 %) for all compounds, with detection limits ranging from to 012 gπl. Conclusion As the analytical procedure does not include any concentration or cleanup steps, it is easy and fast to perform, making it applicable for analysis in pesticides monitoring programmes in milk. Key word : Pyreghrins ; Pesticides ; Hydrocarbons, Chlorinated ; Mass Fragmentography ; Chemistry, Analytical ; Milk 20 60, [2 ] : (2001BA804A BA804A45) : :, [3 ] [4,5 ],, [6,7 ],, [1 ], ( Solid phase, microextraction, SPME) 1989 Pawliszyn,,,,,,, [8,9 ] SPME, [10,11 ],,SPME, ( GC MSD) (SIM) 23 8, ,

2 290 CHINESE JOURNAL OF FOOD HYGIENE ,,,,, QP2010 plus () : Rxi 5MS (30 m 0125 mm 0125m,Restex ) ; SPME,Supelco (Bellefonte, PA, USA),( PA,85m) ;15 ml,,varian ;,Corning ; (Vortex 2 GENIE, Scientific Industries) ( EASY pure R UVΠUF) > % () ( p, p DDE p, p DDD o, p DDT p, p DDT > 99 %) Sigma (St1Louis, MO, USA) ; 8 ( > 98 %) Dr1 Ehrenstorfer ( Augsburg, Germany) ( 10 mirex ; 100 mgπl 6 ( 6 HCB ; 100 mgπl), ( Cambridge Isotope Laboratories, USA) (Fisher ) ( ) ,,10 ml,, ,,, 4 : 2 mgπl, p, p DDE p, p DDDo, p DDT p, p DDT 1 mgπl, 015 mgπl, 4 mgπl mirex 6 HCB ( 100 mgπl ) 016 ml, ml, 610 mgπl, 4 114,4, 1 h ml, 5 ml 5 l 113 g NaCl,, ( ), 20 s,4, 20 min,90 50 min,,260 5 min,,gc MS ;, 110 mlπmin,3 mlπmin ;,1 min (1 min 6) ; : 50, 1 min, 30 Πmin 150,5 Πmin 185, 4 min, 10 Πmin 280, 6 min, min ( EI), 70 ev ; :220 ; :220 ; : kv ; : 1115 min( scan mode),50450 u, [12 ],: (PA,85m),113 g, min,260 5 min , (SCAN), NIST05, (TIC) 1, TIC

3 HS SPME GC MS 291 (11,21,2 1 6,31,41,51,61,71,81,91,101,111,121,131,141,151,161,171 p, p DDE,181,191, 201 p, p DDD,211o, p DDT, 221, 231 p, p DDT, 241, 251, 261, 271, 281, ,291,301,311 ) , SIM,, ( ( %) (t R Πmin) %) Q1 Q2 ( ( %) (t R Πmin) %) Q1 Q2 1 HCH alpha ( ) (100) 183(94) 185(75) 2 HCB( ) (100) 286(78) 288(45) 2 6 HCB( 6 ) (100) 292(62) 294(24) 3 HCH beta ( ) (100) 217(77) 221(50) 4 Linedane () (100) 217(78) 221(48) 5 PCNB( ) (100) 235(63) 239(60) 6 HCH delta ( ) (100) 183(98) 185(34) 7 Chlorothalonil ( ) (100) 264(77) 268(49) 8 HEPT() (100) 270(55) 274(80) 9 S 421 ( ) (100) 132(94) 134(31) 10 Aldrin( ) (100) 261(66) 265(67) 11 Dicofol ( ) (100) 141(62) 250(23) 12 HCE() (100) 351(53) 355(84) 13 Allenthrin() (100) 91(35) 136(24) (100) 91(30) 136(21) 14 trans Chlordane() (100) 371(45) 375(89) 15 cis Chlordane () (100) 371(45) 375(89) 16 trans Nonachlor () (100) 407(98) 411(61) 17 p, p DDE( ) (100) 316(78) 320(48) 18 Dieldrin( ) (100) 261(63) 265 (73) 19 Endrin() (100) 261(61) 265 (67) 20 p, p DDD( ) (100) 237(65) 239 (23) 21 o, p DDT( ) (100) 237(64) 239 (23) 22 cis Nonachlor () (100) 407(98) 411 (61) 23 p, p DDT( ) (100) 237(64) 239 (24) 24 Teramethrin( ) (100) 81(23) 123 (26) (100) 81(23) 123 (50) 25 Bifenthrin() (100) 166(35) 182 (16) 26 Fenpropathrin() (100) 125(83) 265 (48) 27 Phenothrin() (81) 123(100) 81 (32) (68) 123(100) 81 (42) 28 Mirex( ) (100) 270(55) 274 (79) Mirex( 10 ) (100) 275(60) 279 (76) 29 Lambda Cyhalothrin ( ) (100) 141(63) 197 (81) 30 cis Permethrin( ) (100) 163(20) 165 (18) 31 trans Permethrin ( (100) 163(28) 165 (27) )

4 292 CHINESE JOURNAL OF FOOD HYGIENE ,5 ml l31, 5 l 10 mirex 5 l, ,3 0198, SΠN = 3 (LOD), LOD 13 C 6 HCB,p, p 012gΠL,01002gΠL 2 DDD 6, 214, , 2 l40 l( LOD ( gπl) ( gπl) 2 ( n = 5) R ( n = 6) ( n = 6) ( gπl) ( %) ( gx RSD) ( gπl) ( %) ( gx RSD) y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = 9189 x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x y = x

5 HS SPME GC MS 293 2,2) 5 l ( 016gΠL),,, 2, 70 %120 % 3 31 HS SPME,,,,,,,,, [1 ]. [M]. :,2003 : [2 ]. [M]. :,2002 : [3 ] APLADA2SARLIS P, LIAPIS K S, MILISDIS G E, et al. Study of procymidone and propargite residue levels resulting from application to greenhouse tomatoes[j ]. Environ Contam Toxicol,1994,52 :135. [4 ] GRETCH F M, ROSEN J D. Automated sample clean2up for pesticide multiresidue analysis[j ]. Assoc Off Anal Chem,1987,67 : [5 ],,,. [J ].,2004,22 (5) : [6 ],,,. 44 [J ].,2005,33 (2) :290. [7 ] JONG2KI HONG, HYE2YOUNG KIM, DO2GYUN KIM, et al. Rapid determination of chlorinated pesticides in fish by freezing2lipid filtration, solid2phase extraction and gas chromatography2mass spectrometry[j ].J Chromatogr A,2004,1038 : [8 ] PAWLISZYN J. Sample preparation : Quo Vadis [ J ]. Anal Chem, 2003,75 :2543. [9 ] BELARDI R G, PAWLISZYN J. The application of chemically modified fused silica fibers in the extraction of organics from water matrix samples and their rapid transfer to capillary columns[j ]. Water Pollut Res J Can, 1989,24 :179. [10 ] TOMKINSA B A, BARNARD A R. Determination of organochlorine pesticides in ground water using solid2phase microextraction followed by dual2column gas chromatography with electron2capture detection [J ].J Chromatogr A, 2002,964 : [11 ] NATALIA CAMPILLO, ROSA PENALVER, NEREA AGUINAGA, et al. Solid2phase microextraction and gas chromatography with atomic emission detection for multiresidue determination of pesticides in honey[j ]. Anal Chim Acta, 2006,562 :9215. [12 ],,,.. [: ] :R15 ;TQ ;TS25211 :A : (2007) (WHL) 5 17, 10 8,,,,,,, 2002,,;,20 % ; ,35 %,30 %, 2002, %, 116, %2002,2218 %,711 %, ,1992,39 %, 97 %, 1816 %,116

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