SNT 3032-2011 出口食品中三聚氰胺和三聚氰酸检测方法 液相色谱-质谱质谱法.pdf

S/T 3032-2011 Determination of melamine and cyanuric acid in foodstuffs for export-HPLC-MS/MS method 20 11-09-09 1li 2012-04-01 SNIT 3032-2011*fUtcJm GB/T 1.1-2009 ili(l9f;W.Jjltlti1tt.irtt:t tf:*X f4 I*J iiJ lk *J I*X f4 1.tHJL/f*t!l1JtIJJ!:*J Jifff 0*mwooilin.;.fi:,Jg:l;tifiL:rflA-niLt.iliA:lJtJfqi,rl1:tliiJF-9J$A jjllt1JAgcf.0,9J$AJtili.AJJ6J.J.4-?f-if1A:,-$ltzf,tlj 74.1$/fW.,flj BB,hktl-,jtJ5,*1 ttl D it l:f:J.:.IJiO=-ltm W!tl n-51i ffl*ts tt-J9i it 1 J9i it 51i SN/T 3032-20 11*rM-=ammm-m;a*fiT-?fEm=tm,m-lff-It,Jfh-&,tf-,E-E,m E:i-ji-,:J1i;L,trmf,.WHIB lJj(fJUfi;Jl1 t)t T r:j I _J .iltf rl:IU!Hu.:Jlll.J iBHH Z.dMBii,.IJ(r 5t.l-11 iiMt 1t-.3.1 3.2 3.3.ii c.:til,fJ;if rJl 0 3.4 l:fHsii.3.5 t1 At.3.6 it:mz.3.7 fll:.3.8=Z.JJJ(.3.9 l.tl-;j(7-3,YI+Yz):lit 3.10 Z.Jffl r-7)(5+5,V+V2)d.llfJ(500 pH:2.03.0,Z.!ilt!Jj.fG -Jlli i1t I Jlli itH?J!UIH/(f iiE.tf-3.11 1 mol/Llitlfl:Xf.Tlftflt 83 mLJtififl(3.6)Jfj*j!J 1 L.3.12 5%l7JEf:IM:tit:ITR 95 mL lflm:5 mL*.m1:J.ffldifftGJ.3.13 100 mmoi/L rpmzfi-t L.ati0+9,Y_+Yz)pH 3.2 m:fiHiftJJJtt 6.3 g!lftf.J(3.5)ifjfrt=f 100 mL!4!7)(9=J,1JO.A 900 mL Z.Hltn!,_m ff1 ltTr pH 3.2:r:O.1.3.14*0.I%rpMtJJL.!fii:M 1 L L.HtJ,)Ju.A 1 mL fl3M.t!t6-J.3.15?l!fmJ!:-fit.It:!(melamine,CAS:108-78-1),_ J1J(Iii fL 1 p;j.f;f-C5 N3-melamine,CAS-g:2874 76-11-3),_ ft Ml(cyanuric acid,CAS%:108-80-5),_ At fii 1:l P3 (3 C3-cyanuric acid,CAS-:201996-37-4),ttllt:lt9)(r 98%.3.16*F 1ff.-fib tfl:?jjlj fit lDfl ffF II)=Jfl(=It&tiL P-J.f;f-(lJ tr-?llfit(3.15)0.1 g(lDfl jlj 0.000 1 g)JH L.n;+;J(3.lO)mM fil;Jt r 100 mL iJ JfR I I?)J1Jife$fJ.Ql(;JtijJl 19 1 mg/mL aJ.f;?lmtfl.lll&ftl1!i+:ftmtP,-18-c F M#.?jIJfffllk=Wt:rtt-=,_ fnj*P3 aJ J1 C3.15)0.1 g(f;lfifi!J!J o.ooo 1 g).JH ry-ft:.=.L.lf!it-f*:ff.3.17 liE fBJ-fm.jfHl:?ftf9llltk 100 11L.t*llf_.ril-T 100 mL iiHiirtt,ffl L.BW,jlj IC.llt 1 11g/m L aJ.:Jllt H1i,.:Jft tU:,=1BJt fRJ ill:P3 f,j i;J.&-Jl it ftllfi-fiL:l P3 t;j 5 1fE m-tit,it mmrcititJ.:rg:fimtr:?,-1s-c v;,-r ii:Ytf.3.18*Flff.T.fF!ltl:?JEf$Jlk:i:J:1!E4 rBJ-fl#_.m-3.1n.ro z:.m fll mr 3.13)JCfliiJ:ifi Jj(A91!-fr5ItF rtll ritil,ttMJ.Jr!I1f:l!l:-1 10 ng/mLsoo ng/mL,=Jl 11t Friltil P-15 t-ti JJ;J.J 100 ng/mL,_JHllt FriJtil pgt-&13.1.1 zoo ng/mL,tlaiiiHt-tAC.3.19 1Llm:O.22f-tm,;f;fJL.3.20 Anpelclcan MCT 1t Anpelclean MCT tt:l!t i1Cif*f;j-!-)(31f llfH ilEJTFF a.!Uti HH$.tiH!-.GLm:JJ T*at 3!-F (19 V.111 SNIT 3032-2011 Z.Mf,Jtlod:PbllA 10 mL Z.Mf-r7JC3.9)rEff!fi 30 s,N:fJOA-tt 1 mol/L!t:MHiJ?ilL 5 mm,JikJ:TN T 50 mL!1!.MC.ifP,jJOA 5 mL Z.!Wt1gfllifBt,.itim-fr 2 min,1 C F 8 ooo r/min AI L 5 min,if c.ffil:i:ttJUfL(tJU1LBi1tffJZ!i1+7(3.10)ifilMJcil&2 mL T 15 mL J&JMf-P,1JoA 0.8 mL r 7J,.ffi Z.Jfff+l(3.10)5 mL,1t.6.1.2 ;f8:mc.ftg 19J:tf l g(f9fl 0.01 g).It-T 50 mL-*4 L I,?t U1Jo A 100-tL aJ=me lfifti.1(3.17)200-tL JlJ _JkfUI lfiJ iiL#f,f-1(3.17),1JOA 8 mL Z.mt+7.1(5+5,V,.L Vz)(3.10)nt 30 s,.pJ:boA-:lM:1 mol/L tklttfHO.11)-pH 2.o-3.o,:Milt 2 min,til pi 15 min,8 ooo r/min.C.5 min.J:Wiillnil!tiiUitfi!i)t.lfiZ.Jm+-7.13.lO)mJr 15 mL J&i.l 1f,Jlj GJYj.J.;(3.10)-lf!J 8 mL tr.ti,:f#$1-t.6.1.3 fllJ.L$1.-*il,RPJ lliO:&JJ.MJ;d:2 g(fitftl o.01 g)r 50 mL*1-Lft,1JoA 2 mL-*7l!.Y7.1,200-tL aJ=Jlt(rniL.P3 tJ;m1fl(3.17)f:U 100-tL 99=Jll(Btl fii.ltr m 1ll(3.1 7),.bllA 4 mL Z.BW,i;ij:ttftm 30 s,.f11.1JOA-1 mol/L!tftt1l(3.11)-;l pH 2.0-3.0,7MrEn!1 2 min,Sf.F 15 min.4 CF 8 ooo r/min L 5 min .t tflif:Utt r btJ!Gffl z.nR-(3.10)lfiJM J-T 15 mL J&J;t!N tf:t.J:M G Brl-7(3.10)ff8mL:/i:.tfiL Jtltf.!lli:a:fF 1 gC:mfif 0.01 g),Jt-=f 50 mL Wi*4/fJC.rl1,?j-jjrJ.bUA 100-tL(tJ_.J!ti!li.lfiL P-3til(3.17);fft 200 t-tL(!J-!iiUz.tFm (3.17),ffl 3 mL 77.1 rifM.110 A 7 mL Z.JJR,m 30 s,-Pf.bllA-):Eit 1 mol/L fi!lfHC3.11)-pH 2.o-3.o,:MEm 2 min,iffifl.i 15 min,4 c I-8 000 r/min L 5 min.:toJilb,:to)mf,t)Ffgf-fffl 5 mL Z.lm.iEBMB!i.l:l:J:tmtlt._tlltltBtstJH G!n+;j(3.lO)?fFJmJ.li 2 mL=f 15 mL.Jj!J 11 rJl,JJUA 0.8 mL -TJJ.ffl G.Jm+7(3.10);J$5 mL ti.:ti.)!)1t.6.2;qtt MCT tml&.flttl!t.lma.19)frT,ril#!la-/.Mif-&:il!n.6.3 001 6.3.1.1 if#:HlLIC B;OSO mmX 2.1 mm,5-tm),Mffi i.6.3.1.2 ii!t:A:IOO mmol/L lflll+Z.Jfft0+9,V+Vz)pH 3.2;B:O.l%lflftt(!JZ.Jfi*i,J3t ti:.lm fV!A!.1 3 SN/T 3032-20 11 a-t IBJ 100 mmoi/L lllMit+GJM(l l-9,*o.1 Yo m(!J GJm mm 0 2.5 4 8 8.5 12 6.3.1.3 int:0.4 mL/min.6.3.1.4:i!l:*fit:10 J.LL.6.3.1.s.ttm:?l11fil.6.3.2 l.iil.ftf 6.3.2 1-T:IfJtJfESI,Jl:V,+Vz)pH3.2tilt;IJ;fft A)0 0 100 6.3.2.2 m1nt:$&J.iil.00:MRM.6.3.2.3 t(GSl),m mlltrmlJmtntiit 6.3.2.4 fl!lll9J r.t!ff(IS),il CXP)Jiilt1tli:-f!Rfl.ll,6.3.3 jlg *f-(fj*Jt s-t1JtJ.K.lfl,J.iil1gm.juHfHF rfJ f.f fM -tt:iiUlB:t-,=m J.iY(MRM);ifOO!A!.OO B.1.6.3.4 ltDlE Mt.f9 B)100 100 0 0 100 100 19 11 fiB*.iS ec.;19!0*,W gm dlf!A!.t fk A.Q fl!ff(EP),HUt:i:ili J:t r.t!ff itt#,f!F?l tlii I fF J.iii til J.iii iE)(tt J.iii m:fE pg 0 ti Fo 7t .t)15ltH!d4-F,=mz-=Jl1Hffi11E1il$&trcJmiil*Dfg ift-liftil/l!ftiHk1ttrMiit:*f:fn:ftmifF?i,u*ut*F P fM liltaJ m a;j rBJ tl?t.fb f,-!*WI at ISJ;tE 5%Z P3;tt.r aJ;tt:l xif J:l,:Jik ffl;tt:l x-T:liB!il =f:F J:l Yl Jl a 7t It;&71 m.t&Yt *F?ti fF rif oSO%20%-so%l0%-20%10%-ft iff(l9 Ja:*ilt 20%.1: