DB32T 1163-2007 鸡肝中金刚烷胺残留量的测定 液相色谱-串联质谱法.pdf

ICS 65.020.01 B 40:21644-2008 5I DB32 D832/T 1163-2007 f XJIJi;c1mB9!1J1E:i*i-$*i5*Determination of amantadine residues in chicken liver-Liquid chromatography-tandem mass spectrometry method 2007-11-26 15 2008-01-26 lli 0832/T 1163-2007 j TfHjJltJf=9=IlJtftiJH,fg,tltIJAE*+IF(lL*IF1H GB/Tl.1-2000;fIFi1HtI1t-IJ!lJ 1-?1:;fIFitrJ;f5fD;J;.mJlU 5fJ GB/Tl.2-2002.fIF l1HtI fF-Jllj 2 1m?1:;fIF ii 9=I;J;!1l1fdi 15z:*=*J*J?:iJ fiJfl AE 151t=J)Am ltU 0*;ffiiJ ftAAii r4tt ft0*;fii EB rr iJj;&;ftff tJi!:il 0*.fii EB rr iJj;f=)1t1iL;!MiJ9=I JC,l 0*;f/ffilA:ffi;ft,td(*,B1,3im i11,w11,$?:,*m,:r:t,IH4o DB32/T 1163-2007:2l-qlljJliE T 1W;ti;-$J9ti;ltiuiEx%fcp IJ:mJ1t IJJJ:L U iE1J;It,t2 t,f/iTiftJ N;fJ;j.wNo:;t*fffi:ffl-:rx%fcprxJlj;tiGHJ;lt00:i:8:11&U,tb712.0 g/kgo 2 Ji!.mttiJ Iffl3ti!:J:T 7uJtf:j:cp 1J%:imi1:;t*ff(iIJ 51 ffliITi mG71*fffi 8:1%:*)(0 fLa El tAIJ 51 JfJ Jt14,;f-t:MiJ pfi1J.(MIJ).rrAA:m:;tfi,i1ri,B*fiIJ1J:SpHiJljJKJt141J#JTh&*o fLf&aEl t):JtrJ51 ffl Jt1*,jt:ifdifTh&:;t:ffl r*ffliL CB/T 6682-1992 7HJT3r:m7j(Jl*tr;fJiJ.%Z1JZ:3 mIl lA:r4 cp J-l.00 IJ rxJ J:mHW1WJ j;&,jj 12:9:1;t mrot 0imi1 E,-fftMIDHRH$*J9t*,IJ:i&f=i?f:%-=f llii;Altl(S RM)1J:rt:i!iTt2 U0 4.1 i1fIj;fMM,J S;W!JJiJa Il)H,*fffipJTmlAJrU:l$:77J.+JTL!J:iiJrU,7j71)(J7j,11=-g.CB/T 6682-1992CP R7lJliE 0 4.1.1 Ijtt+fffip:L!J:Jt99%o 4.1.2 MtJ*;J;i (*if):L!J:Jt 99%o 4.1.3 i3!J:i;L!J:o 4.1.4 lJjt iL!J:o 4.1.5 lE 2;tiG 4.1.6 HmllW 4.1.7=i3JG 4.1.8 2.5%z:,M7lm1W 4.1.9-l1tfJ(!/f1W(pH1l):fff6.75gJ(1H:m=r 100mLi*7lCP 0 4.1.1 0;1Hic*IJ 4.1.10.1*ffifi1W fjFItZXJIJ;tiG:t:+fffiJfb 10.0mg OMifj O.OOOlg),Jt-f-100mL1t*h 9IfflEj3l mmtHf.fnf:tuJt,tffi Pi0f1ju 100 g/mL IJm1W,itJJ*fffi1*Wo it 4C iH-jC 1iHtA71 3 1-J3 0 4.1.10.2+fffiI fF1W;ffl,&:IIY.*fffifiW 1mL 1 100mL?Jill nacp,:JJo Ej3 w:mffltH;WHf.tIJN,tBf,1f1J 1.0 g/mL*ffiiIfFH,4CWtf-o fiMnm71 11-J3 4.1.10.3 p*ffm1W ItZiC*tJ*ffiiJ=lp 10.0mg(1iffiO.OOOlg),-f-100mLii*aCPfflm mH:ffi*5ttIJN,tffi 1J1o f1jum 100 I.l g/mL mw,1t:71*ffM;i&1W,;4C15iH-jCo fi1+tA:h 3 1-J3;ItZ:-E:1*-?lrM,ffl M:-7l 1ft:liH,JlL Jt(R1$,Wj it-18 C f4 fJd;j-H,t:tJ B J;f4 ffl 0 4.3.2 tJiH)(JfX:1g(0.OSg)it:f4,jlT20mLIHYg,1tn!A:imAEtI Iij:-7.K(SO:SO)20011 L,p;j*;Fm 40011L,-jtttyj#(pHIl)40011L,m;hDmJt(lttEcj:)c-=aEfl;l;1c-Fpg(2.0:2.0:0.1)SmL,1iJVf6lmin,:tJH%10min,liH)5min,5:J-JtR.tmiT-iJ;flfhDAmJtt.u:c;l;1c-EtI;I;1c-Hpg IW(2.0:2.0:0.1)SmL,IpJ1,vdtjf:;H.tFzfmi,J-40 C!JR4:0J,:T,1:HaimhD A 1mL0fLZ9J ru:fH,t!J0fLlf.,:Itt1TLCiMS/MS5:J-;j:JT 0 4.3.3*iF/i;9!IJ;Hs*IJtk JJt(Bt:Nlg(O.OS g)T20mLtt.Il,hDA*iFftEI1t(4.1.10.2)Ei,154.3.2.,&ftEru:,mo 4.3.4;9!IJ 4.3.4.1.HHHl:lttfH:CB,150 mmX4.6mm(i.d);1EZ9Ji:Ej3g+2.5%z:,7.km(80:20)0fLJM:0.6mL/mim;i!H-f.:Ji:2011 L:U:20C o 4.3.4.2:i1*fr7J 0l2t-=f(ESI 11%i);hD1jEllljjL:tJ 320C;1ET7J):tr3m;j&:jf-&lKlYJu(SRM);1i:lEti4:.(Ar)fffJ 1.2mTorr;J:WTfC:i:5:J-*JTt(j+&fZ7H3IJ:tJ m/z l S2-13S(lXJtltt),miz27S-230 OJ(H 1lr)0 tL iiliFf&X1fZa:lEt1tff.lJi!,L:W 1 IXlIJmnrl pg*iFil.*Jls%i:;9!IJTrltIff 1IJ:rtf!;-T-Ti-m.rlli.I f5;1.1PJ m/z m/z eV 152 135 30:3li:JIJ)J1i 152 107 29 15 2 4393 230;jl;Jl 1:iJ.(P;J+5;)27 5 30 ii:*:AfEfi!:l!;r,2 I DB32/T 1163-2007 4.4 jtHtHr1*j 4.4.1;gt1*IJi!Jf 1:r 1 i5J1,Jt!JtZ14F,1,Jt*4 r:p 11ro F5W1ft umij$*iFftEm8%B1 18)8J$JJUt11:f*2 tr-J*,ISJ*UIE1,Jt*4r:p#fr1ftIJmij$y31.0 J:,illlfl J+t X1fUI$*2ffiX1$mftm tX1$,Ij%jti/f iJmLk%!,50 20 2050 25 1O20:;10 30 50 4.4.2;g7J5*1ft Umij$1r11*J:tiFm(*j15:tE EtpmT1-t(EST)7JA-f,-=t1:MM+I-J,f1E:5tf-luI!,-5j3IJ A m/z 152,275 0:jf-ttX1f1E:5tT;TUIHM+Hr:Itt1T=&)Jln:5t*JT,1ftRJIJmij$1r1*jtW:MEJJWh;T:5tJJUA m/z135,230,:5t j3ujt:1t:A fEti:5t*JTB1llfli9lWJf=0 1ftIJmij$IE:;:+l*J:tiFi5Zrr T(1)UITIITtRZ tt:Itt1T 1fLBB)G AftElEiL;fiFf1Ei9lJEm 1D1,Jt;f4YlEmr-&r:p 1ftIH3tij$8J oiDJB1Jtt:):jB11xiftrou;lU1m I*J,13i,llj JT HA 0 1$A(1)itt:1*hJtjRr:p1ftIJmij$EJJij(g/kg):AXAji XVs Xc,X .(I)A.,XAjXm J:t=P:X-mff9JlXJlj:J:fGHiiEr-JJJ,Wf,f7lr,5Vf5(ll glkg)A-l-JtNlYl1jJEm:i1!Z=P lXJlj:J:fGijJE.m?f!;=r-i-dEr-Jdllif;f,H A1-iJt4lYl1jJE mi1!Z=P I*J 1iFtil ifIZ;=r-lYfd Er-J dffii m As-iiF(iUJE mi1!Z=P-it U:J:fG ii JE-m T lEr-J df:j;19Ars-1iF ii)i!lj JE m*=P I*J liF1Q 1E=r-Er-J f:j*9Cs-:tiFrtIIfFi1!Z=PU:J:fGHBi&gLf7l1i!(5J7t(II g/mU vs-frrulffi1!Z!lXffl,tL1:J7t(II U m-iM4 Er-J!IX fthl.!f!flL 1:7:R:(g)1:WUE*1Ifi1r.l12B j.)i!lj iEra ffl.IfL1T;m iE ifJ4l*Iij:):j*j.f fii 3fil:1f:i3 j&:oj;:.5.1 tj *7Jtlxfr:pEJJift8jllA 2.0glkg 0 5.2;i1flm*7J$;1 4.0 g/kg20 g/kg:lJDt,lj*+LiJilt&$mA 60%120%0 5.3 Jl*7Jtt:EJJ:Jtt 1*J:FP!tti!:;15%,:JttlS:FP!ii!x:;15%0 3-D832/T 1163-2007 fl11-IR A(ifintHH-IR)!XlIJ 1ftW;fQ pg f;f-ag;J.i*1fI RT:0.00-8.00 SM 11G RT 1.55 NL:9A9E6 AA:124391385 rrJz=229.50-230.50 F:+c 100sid=-B 00 SRM ms2 275.00-30.00 I80 I 229.9B-230 031 MS Genesis std00160-1 40 20.,0RT:1.27 NL.223E6 AA:23423225 mz=134.60-1 35 60 F+c S1d=-8.00 SRM ms2 152 00-30 00 I,OJ 80 93_ 06-135.13J MS u GenesIs sldOOl3 60.D 40 20.,Q;.-.-=-:=I RT:1.27 tt.3 GE5 AA:3694393 rT.il7.10GoO lUl(Wf 1:100-j$;0=-0 OU SRM,n;,152 OU-30 00 I 80.,;3 oa u.13J MS Grof:o;!s(W00 1 6040;20-0-_ RT:1.27 NL_ 1.98E5 AA:2021975 rrJz=92.60-93.60 F.+c sid=-8.00 SRM ms2 152.00