( Pht halic Acid Esters, PA Es) PA Es
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1 21 6 Vol. 21 No. 6 J OU RNAL OF ANAL YTICAL SCIENCE Dec : (2005) ,2, 3 2, 2, 2 (1., ; 2., ) : ( ), : ; ; : TQ :A 1 ( Plastizer),, ; [ 1 ], ( Pht halic Acid Esters, PA Es) PA Es,, ( PVC), 50 % [2,3 ], [4 ], (22 ) (DEHP) (DOP) [1 ] PA Es (DMP) ( ) , 8 [2 ] PA Es [5 ],DMP ( ) DEP ( ) DBP ( ) BBP( ) DNOP ( ) DEHP( 2(22 ) ) ( EPA) [ 6 ] DBP BBP D EH DNOP DIN P ( ) DIDP ( ) 6, 0. 1 % [7 ], PA Es, ( ),, 8,, : D EH BBP DBP DCHP ( ) D EP DN PP ( ) D H P ( ) DPP ( ) [7 ] 2 PA Es,, PA Es,,,,, h, [2 ] 2. 1 PA Es [9 ], [9 ] [10,11 ] : : 687
2 6 : 20,, ( HPL C),,,, ( ),,,, 100 m, [ 11 ] [12 ],,,, [11 ] ( m), (10 40 m) PA Es, ;,,,,, 2. 2 PA Es, 10-9, [13 ], PA Es 2 (LL E) [ 14 ] ( SPE) [15-20 ] (SPM E) [ ] (SM E) [26 ] (SBSE) [ 27 ] LL E, PA Es,,,,, SPE LL E,,,,, SPE2GC2MS [18,19 ] SPE2L C2MS [19 ],,,, ;,,, SPM E, 90, SPE, SPE,, [21 ] SPME2GC2MS PAEs PAEs SPME,,, PAEs, ;,,, g/ L ng/ L [26 ] (1 1) PA Es, C18 PA Es SBSE ( PDMS), ( P TV) PDMS SPM E,,SBSE 1 000,SPM E 100 Pegalver [27 ] SBSE GC2MS,, PA Es 10 ng/ L 2. 3 PA Es, 2 ( Kow ),,, [28 ] PA Es,, 2,, PA Es, [29 ], / (3/ 1,V / V ),, H PL C PA Es,, % %, PA Es 688
3 PA Es,,,,, ( SSL E) [30,31 ] [32,33 ] (M E) [34 ] (SFE) [ 35,36 ] (ASE) [ 37 ] 3 PA Es,,, PA Es [ 10 ], ( GC) (L C) ( IR) (NMR) ( TL C) PA Es [2 ], ( FID) ( ECD) (MSD) [4 ] 2, HPLC LC2MS 3. 1 ( GC) GC HP25 DB217 H T PA Es,,, ( DIN P DIDP ),,,, GC2 MS, ( SIM),, m/ z [ 38,42 ] 1 PA Es GC Table 1 Analytical methods for determining PAEs by GC Sample matrix Analytical method Preparation method Detection limit Ref. Indoor Air GC2MS Adsorption with charcoal tube, pg [12 ] GC2FPD Extraction by ultrasonication Water samples On2line SPE, Elution with ethyl acetate ng/ L [18 ] SPE2GC2MS Landfill leachate GC2MS Extraction in Soxhlet with 2 [ 20 ] dichloromethane and n2hexane ; SPE and ion exchange chromatography Seawater GC2MS SPM E with 100 m PDMS g/ L [21 ] Water GC2ECD SPME with polyacrylate fiber g/ L [22 ] Water samples GC2MS SPM E with 85 m polyacrylate fiber g/ L [23 ] Water samples GC2MS SPME with 30 m PDMS g/ L [24 ] Water samples Large volume Stir bar sorptive extraction (SBSE) g/ L [27 ] injection GC2MS PVC products GC2MS (SIM) Liquid2liquid extraction with ng/ g [31 ] Human saliva ethyl acetate, clean2upusing florisil column chromatograph PVC Plastics GC2MS( SIM) Ultrasonic extraction with chloroform 10 mg/ kg [ 33 ] PVC GC2FID Microwave2assisted extraction 2 [ 34 ] with methanol Water sample GC2MS Methylene chloride Extraction ng [38 ] Sediment sample PVC toys GC2MS Extraction with dichloromethane g/ L [39 ] Childcare articles 3. 2 ( LC), ( HPL C) 2 (L C2MS) H PL C2UV 689
4 6 : 20 C8 C18, 2 2 ; L C2MS PA Es C62C10, GC2MS,, GC2MS L C2MS,Lin [2 ] L C/ ESI2MS GC2MS PA Es 2 PA Es Table 2 Analytical methods for determining PAEs by LC Sample matrix Analytical method Preparation method Detection limit Ref. Water samples LC2UV (280nm) SPE with polystyrene column g/ L [17 ] Textile Wastewaters LC2A PCI a 2MS LC2ESI b 2MS Landfill leachate IPC c 2ESI2MS Sediment s, fish L C/ ESI2MS Homogenate,ultrasonic Sequential SPE (SSPE) g/ L [19 ] Extraction with DCM/ Hex (1 1 v/ v) ng/ g [2 ] PVC packing HPL C2UV (270nm) Extraction with hexane ppm [ 30 ] Parenteral nutrition, plasma Intravenous solution HPL C2UV (202nm) Extraction with hexane, column2switching LC2MS Organic layer separation, dry Waters Oasis HLB extraction column 20 ng/ ml [40 ] g/ L [41 ] Notice : a APCI means atmospheric pressure chemical ionization ; b ESI means electrospray ionization ; c IPC means ion2pair chromatography. 4 PA Es : (1) PA Es, GC, PA Es, ; (2) PA Es,, PA Es ; (3) PA Es,, ; (4) PA Es, ( DIN P,DIDP), PA Es,, PA Es, PA Es,PA E : [1 ]. [J ],1997,5 (3) :51. [2 ] Lin Zhong2ping,Michael G I et al. Environ. Sci. &Technol. [J ],2003,3 (6). [3 ] Aignasse M F,Prognon P et al. International Journal of Pharmaceutics[J ],1995,115 :241. [4 ],. [J ],1995,14 (5) :17. [5 ] Cameron George, Harry Prest. Agilent Technologies[J ],2001,3 :1. [6 ],. [J ],2001,21 (4) :362. [7 ],. [ M ]. :. [8 ] Oko2Tex Standard 100 [ S],Ausgabe [9 ],. [J ],2003,19 (1) :108. [10 ]. [J ],1998,14 (6) :21. [11 ],. [J ],1995,23 (12) :1425. [ 12 ] Takamit su Otake,J un Yoshinaga, Yukio Yanagisawa. Environ. Sci. Technol. [J ],2001,35 :3099. [13 ],. [J ],1998,1 :
5 6 20 [14 ] Law R J,Fileman T W,Matthiessen P. Water Sci. Tech. [J ],1991,24 :127. [15 ],,. [J ],2003,3 :66. [16 ],,. [J ],2002,18 (3) :177. [17 ] Jara S,Lysebo C et al. Analytica Chimica Acta[J ],2000,407 :165. [18 ] Brossa L,Marc R M,Borrull F et al. Journal of Chromatography A[J ],2002,963 :287. [19 ] Monserrat Castillo,Dami Barcel. Analytica Chimica Acta[J ],2001,426 :253. [20 ] Iraj do Nascimento Filho,Carin Von Muhlen et al. Chemosphere[J ],2003,50 :657. [21 ],. ( ) [J ],2000,39 (3) :54. [22 ] Gabriela Prokicpokova, Kate rina Holadov,Jan Poustka et al. Analytica Chimica Acta[J ],2002,457 :211. [23 ] Pegalver A,Pocurull E,Borrull F et al. Journal of Chromatography A[J ],2000,872 :191. [24 ] Cortazar E,Zuloaga O,Sanz J C et al. Journal of Chromatography A[J ],2002,978 :165. [25 ] Pegalver A,Pocurull E,Borrull F et al. Journal of Chromatography A[J ],2001,922 :377. [26 ],. [J ],2000,20 (2) :146. [27 ] Pegalver A, Garc a V,Pocurull E et al. Journal of Chromatography A[J ],2003,1007 :1. [28 ],. [J ],1982,6 (1) :461. [29 ],. [J ],1996,10 (2) :15. [ 30 ] Aignass M F, Prognon P,Stachowicz M et al. International Journal of Pharmaceutics[J ],1995,113 :241. [31 ] Tatsuhiro Niino, Tohru Ishibashi et al. Journal of Chromatography B[J ],2002,780 :35. [ 32 ] Bart Tienpont, Frank David, Freddy Vanwalleghem et al. Journal of Chromatography A[J ],2001,911 :235. [33 ],,. [J ],2002,30 (3) :289. [34 ] Cano J M,Mar n M L,S nchez A et al. Journal of Chromatography A[J ],2002,963 :401. [35 ] Mar n M L,Jim nez A,L pez J et al. Journal of Chromatography A[J ],1996,750 :183. [36 ] Mar n M L,Jim nez A,Berenguer V et al. Journal of Supercritical Fluids[J ],1998,12 :271. [37 ],,. [J ],2003,19 (2) :179. [ 38 ] Matteo Vitali,Cattedra di Igiene Ambientale et al. Environment International[J ],1997,23 (3) :337. [39 ] Earls A O,Axford I P,Braybrook J H. Journal of Chromatography A[J ],2003,983 :237. [40 ] Kambia K,Dine T et al. Journal of Chromatography B[J ],2001,755 :297. [ 41 ] Koichi Inoue, Tae Higuchi, Fumio Okada et al. Journal of Pharmaceutical and Biomedical Analysis[J ],2003,31 :1145. [42 ] Castillo M,Barcel D. Trends in Analytical Chemistry[J ],1999,18 (1) :26. Development of the Analysis Methods of Phthalate Plasticizers FAN G Li2ping 1,2, N IU Zeng2yuan 3 2, CA I Fa 2, SUN Jian 2 (1. College of Chemistry and Chemical Engineering, Ocean University of China, Qing dao, S handong ; (2. Qi ng dao Ent ry & Ex it I ns pection an d Quaranti ne B ureau, Qi ng dao, S han don g266002) Abstract : In t his paper, t he develop ment of t he analysis met hods of p ht halic acid esters has been int roduced in detail s. The p reparatio ns of enviro nmental samples ( such as Air, Water, Soil ) and polyvinyl chloride product s have been reviewed. The problem and progress in their determination have also been proposed. Key words : Pht halic acid ester ; Enviro nmental samples ; Polyvinyl chloride ;Determinatio n 691
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