资源描述:
《BJS 202103 蜂蜜中链霉素和双氢链霉素的测定 液相色谱-串联质谱法》由会员上传分享,免费在线阅读,更多相关内容在行业资料-天天文库。
!"#$%&'(犅犑犛202103)*+,-./01,-.23456789:;8(20210113<=>?@ABCDEFG<=
1犅犑犛202103!"#$%&'()$%&*+,-./012304156!"#$%&'()*+,-./*+,0123456748%"#。!"#9:;'()*+,-./*+,08%。278<:=>?@A0BACDEF1GHIJ)0*+,-./*+,,KLM-NOP,HLBQ2RHSTUVWXY,:12345674Z[8,\]#%^。39:';<_`a$%\,b:Icdefgh,iejkGB/T6682$%0lmi。3.19:3.1.1@n(CH3CN):34h。3.1.2op(CH3OH):34h。3.1.3oA(HCOOH):34h。3.1.4>?@A(Cl3CCOOH)。3.1.5BAq/r(KH2PO4)。3.1.6si(NH3·H2O):=^e25%~28%。3.1.7/tWu(NaOH)。3.29:=>3.2.110mol/L/tWuF1:vH40g/tWu(3.1.7),:iFw,xyz{|P,%}z100mL。3.2.20.5mol/L/tWuF1:vH2g/tWu(3.1.7),:iFw,xyz{|P,%}z100mL。3.2.3GH1(=2%>?@A0BACDEF1):vH20g>?@A(3.1.4),~400mLiFw,vH6.80gBAq/r(3.1.5)~z>?@AF1),~400mLiFw,P,:/tWuF1(3.2.1-3.2.2)pHz6.8,~i%}z1000mL,P:。3.2.4F1:fH2.0mLoA(3.1.3)-5.0mL@n(3.1.1);100mL}^),:i%}z100mL,P:。:。3.2.52%sW@n:H2.0mLsi(3.1.6);100mL}^),:@n(3.1.1)%}z100mL,P:。:。3.2.60.5%oAF1:H2.50mLoA(3.1.3),:i%}z500mL,。:。1
2犅犑犛2021033.3?@A3.3.1A*+,](C42H84N14O36S3,CAS:3810740,2f7^1457.38):K¡¢£]¤7¥0]¤7。3.3.2A./*+,](C42H88N14O36S3,CAS:5490277,2f7^1461.41):¦K¡¢£]¤7¥0]¤7。3.4?@B-*=>3.4.1A*+,]§1(1mg/mL,¨*+,©):vH62.6mgA*+,]¤7(ªz0.01mg);«¬),:iFw¡®z50mL}^,¯P:i%}z°±,,²7^³±e1mg/mL0]§1,-18℃´µ¶·,a¸¹6º»。C1:¼<:½¾¿À0]¤7,ÁTU2f7^ÂÃPTU]v^。C2:¼KÄÅ:,ÆÇÈ]§1fɲ«ÊÉ,ËÌÈ«ÊÉwÍÅ:。3.4.2A./*+,]§1(1mg/mL,¨./*+,©):vH62.6mgA./*+,]¤7(ªz0.01mg);«¬),:iFw¡®z50mL}^,¯P:i%}z°±,,²7^³±e1mg/mL]§1,-18℃´µ¶·,a¸¹6º»。C1:¼<:½¾¿À0]¤7,ÁTU2f7^ÂÃPTU]v^。C2:¼KÄÅ:,ÆÇÈ]§1fɲ«ÊÉ,ËÌÈ«ÊÉwÍÅ:。3.4.3k]F1:H1.00mL*+,]§1(3.4.1)、1.00mL./*+,]§1(3.4.2),Î;Ïl10mL}^),:iÐÑ¡%}z°±,,²7^³±e100μg/mL0k])Ò1,0℃~4℃´µ¶·,a¸¹1º»。3.4.4k])ÒF1:È*+,-./*+,k]F1(3.4.3),:iÓmÐѲ7^³±fe10.0μg/mL、1.00μg/mL、0.100μg/mL0k])ÒF1。:Ô。3.5;<3.5.1Q2RHS(60mg,3mL):犖@ÕÖ×ØÙÚ-q@ÕÖÛÜiÜÝÞßàáâ¦2ãä。3.5.2%^Oå。3.5.3æçOè:aé2(êë),çì0.22μm。4DE'FG4.11234>íîïð5674Z:añòóLô(ESIô)。4.2ñõÞ:ö^fe0.01mg-0.001g。4.3÷øùúû。4.4üýþÿû。4.5LMé:®!"#;8000r/min。59H>GIJK5.19H*>G$%&0'({J,Ƚ)*d。a%&0J,[(,+,-./0,Î;"üN60℃0i1)|2,ùú,3J456WP),f70.5kg8eIJ,É9V}û),:!xyz{|,,;¡]<。2
3犅犑犛2021035.29H*JKÈIJ;Ä|0¶·。6LMNO6.1PQvH5gIJ(ªz0.01g);50mLLM=),~10mLGH1(3.2.3)÷ø1min,üýGH15min,H7P,ÈF1®z25mL}^),:9^GH1(3.2.3)>LM=,k¡>1z}^),:GH1(3.2.3)%}z25mL°±,,®z50mLLM=),8000r/minLM5min,ÿ13:。¼J)a?^@A,B:%^OåNO,CD¯E05mLO1,FYGHO13VW。6.2RSIÌ:3mLop、3mLiJWQ2RHS(3.5.1)。H5.0mLÿ1¦O1(6.1),¨"K;1mL/min0L!45MNQ2RHS,CDL71;:iNOÌ,ËÌ2mL;È«SPQ,~1.0mLF1(3.2.4)TU,R1SL!"üN1mL/min,FY451。:sW@n(3.2.5)%}z2.0mL,P,KæçOè(3.5.3)NO,T12345674Zfg。6.3T3UV?@B-*>GvHK74"=*+,-./*+,0UV'(J5W,ËW5g(ªz0.01g),f~9^k])ÒF1(3.4.4),²*+,-./*+,=^de5.00μg/kg、10.0μg/kg、20.0μg/kg、50.0μg/kg-100μg/kg0Ö7J,½HX6.1-6.20YZ[8\²,]8I17^³±fe2.50ng/mL、5.00ng/mL、10.0ng/mL、25.0ng/mL、50.0ng/mL,¦ä^_Zû`]a'b./9ã³±cd0]ef。6.4+,WX6.4.1YZ-./0WXgh1234ijk0:a)34S:SIELCObeliscRlLmn34S(opqArÖs)(150mm×2.1mm,5μm),¦Vt2ãä。b)Lu2:Ae@n(3.1.1),Be0.5%oAF1(3.2.6),v±ijwx1。[1\]^_`ayÒ/minLu2A/%Lu2B/%075250.575253.845555.045556.010903
4犅犑犛202103[1()yÒ/minLu2A/%Lu2B/%8.510908.6752514.07525c)L!:0.3mL/min。d)S|:40℃。e)TJ^:5μL。6.4.2YZ30WXgh74ijk0:a)Lô:ñòóLô(ESIô)。b)[8"À:z{]|8(MRM)。c)}~"À:LÀ}~。d)ñòóñ:5500V。e)óWû:344.7kPa(50psi)。f):137.9kPa(20psi)。g):344.7kPa(50psi)。h):55.2kPa(8psi)。i)Lô|±:550℃。j)Oºîïðd<:7^f。k)óW、、、deKh,Å:]SL^¨Å74±[8。%VL、%^L、yÒ、Dñt^wx2。[2$%&'()$%&*30YbL%^LDñyÒtWk¤(犿/狕)(犿/狕)VmsV582.0/263.049*+,582.0/263.0220100582.0/246.043584.0/263.049./*+,584.0/263.0220100584.0/246.041C:6.4.2074ijTgh,ã<:"Ï74Zûy,ZûgBt·+,8%]È74gW¯。6.4.3?@cdef>d+Zû¯8ij0,*+,-./*+,0Ö7k]F1(6.3)TU8%,¨Ö7k]F1³±e],¨¡¢£e¤],¥]8ef。*+,-./*+,0z{]|8(MRM)34¦gw§¨A)0¦A.1。4
5犅犑犛2021036.4.4,ghiX©6.4.1-6.4.20ij8%IJ-Ö7k]F1。IJ)ª]Wk¤034¡¶yÒaÖ7k]F1¶yÒ2«¬,Wcd+±2.5%®¯。IJ)ª]Wk¤0OºL]7Ô,ÏlWk¤,IJ)ª]Wk¤0OºL02°±a³±2ã0kÖ7]±F12«,½²³´"üNx3$%0cd,µB¶·J)·+]0ª]¤。[3,ghij.klmn]*opqrst2L°±犽/%犽>5020<犽≤5010<犽≤20犽≤10²³02´/%±20±25±30±506.4.5,u+,IJ)38¤0`]d]+]ef0fVcd¯,¼=^ü7fVcd,Áí¸~]8Ö7k]F1,ÈIJaÖ7k]F1ÏYÐÑPé8%。*+,、./*+,0¹~³±ÞdºF»0'(_gw§¨B)xB.1。6.4.6vw9x_"~IJ\,dXIJÏ#[8。7yz{|J)*+,-./*+,0¼^XÀ(1)©Ã:犡犻=ρ犻×犿犞×犳…………………………(1)À):犡犻———IJ)38½f犻(犻=1,2)0=^,eæ¾Ë¿¾(μg/kg);ρ犻———À]8efÁ0Â8½f犻(犻=1,2)F17^³±,eþËÄÅ(ng/mL);犞———IJF1¯Æ%}S£,eÄÅ(mL);犳———IJNÇ)0ÐÑÈ;犿———vJ^,e¾(g)。8%%ɨíÊVij0ËÁ0OÌÌÍ8%%É0ÃÎÞdxÏ,%ɶ>a¸Ð。©Ã%É]Ñ_ÒÓ。8+,yz*[}犡=犡1+犡2…………………………(2)À):犡———IJ)*+,a./*+,Ô^,eæ¾Ë¿¾(μg/kg);犡1、犡2———IJ)*+,-./*+,0=^,eæ¾Ë¿¾(μg/kg)。!"#*+,/./*+,0¼^8%%ÉÕ*+,-./*+,¼^®-。5
6犅犑犛2021039~+4*]、@h]、]9.1]ãvJ^e5gy,!"#)*+,-./*+,08%0[7Öde2.0μg/kg,%^Öde5.0μg/kg。9.2@h]!"#+5μg/kg~100μg/kg¹~³±cd¯,ºF»e80%~120%。9.3]+íÊVij0ËÁ0OÌÌÍ8%%É0×"ÁüNÃÎÞd015%。6
7犅犑犛202103犃(8犅犑犛202103犅(º³±iÞ0~]ºF»I(,˺³±iÞÞU8%6Ì,ºF»2]´0I(_wxB.1。[犅.1$%&'()$%&*.k?@st*9xb~]iÞ/ÙÚ'(Û@'(Øi'(Wk¤(μg/kg)ºF»/%RSD/%ºF»/%RSD/%ºF»/%RSD/%5.0090.25.6886.91.6792.25.18*+,20.096.46.9097.36.05111.73.08100108.26.52109.14.79110.53.395.0094.04.8693.32.8897.52.34./*+,20.0104.03.72103.31.66109.33.16100113.22.13113.01.23111.33.24!"#ÜÝÞß:àáâãä[(åæç。!"#(:èéêãë4|R-ìíîï)M、ðê7^|ñ[(òÎåæç、îóâãä[([8ç、ôõãWö[(b、ðêãä[(b。!"#÷Þßø:ùú、ûüü、ýþÿ、!"、#$%、&'。8