【行业标准】 进出口蜂王浆中林可酰胺类药物残留量的测定 液相色谱-质谱质谱法

中化人民共和国出入意检验检按行业标准SN/:2576-218
进隆王林胜腰类
药物我留空的测定
液相色谁·质/质谐法
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家麻怡验
效码防伪
金品伙伴网ht
2010:12-4: 8:
4RA5MY
本标理控照G：！2009给出的双用A全商
本标准中国家认证认订监保管品公中本标淮山中华人民具知国新江山入缆格险份届负黄北单本标要是单人谢文，陈你十报通，http：//foodmate.netSN/T2576--2110
液相产湾微微/服谐法
SN/T 2576-20110)
不标维现滤广那降十将中标可能胺类影齿超品制定的制雅和服柜色语质谱/质说测效方视
本标准适市「降主燃中林需素，氯林可系和呕利标素简益的测众。规施性出用文证
下翁义件对本支件的启用是必不少的，是注！期的用安科，仪汁川期前版适！丁不支七用好小注期的可实件：就最新版会位范乐台的修收单证品丁术文件。GT6S法分价实监宝开水期络和试验有法3法提要
H果醇沉淀样品十质：主消漆加律格点冲济液释端府，C。国布器取小杜净化，液和色游质据/惠谱测，女标法量
微剂和材料
除另有题是外，新成剂均为分新纳，水为（一2期定的一级水。41略：高效报相化谱级
中醇：高效液色段
中酸：高效激防仙端级
501氧食让钻落液：称：热销单品本稀释至114甲照水溶液中醇，本积
质股热缓冲浴液，浴释3送.消m.水中用C1证/氢氧化筑深装调节落液制敏片H水精
H你川#（tiommhlodemonhda，CAsNo.8s918，分了fNxH标准品：纯人等领林端素者骏clindamyeinhyirollorileCA5人0.216%39分了式11你有品纯购大等94.5%.批利得素酸益nrbioyainkydroeh.onceCaN.分，，cNO.Sxo标雅品度等85.4。
儿林时解案、氣权川想京味礼欲南机礼留舒的流：别微取经折篇点草标准品（4.分别醇浴解穿m率波浓度为箱像存有效圳个htt
S/F2576-2010
4。10空样件提最装：用不含林可胺半约按为降1浆羊出按照第？章副备空由群品溶液，411标准工价溶液：根据靠热用室产品落（1心）将你销备液释成浓度公ng/mI.Sg/mt.1og/L.ng/mc时含标准作溶液，相当于样品中含有2/k5ug/kg.icg/kg.53u/kg.1rpnu物412C固相举取小在30s.3ml或进，俊前依次用5r中尊5ml求预洗.4.13微孔滤膜：.45有机
议器和设备
额相色谱-谱/质费：配有电质家离“源（认）。5.2天：最为0.918租6.35
5.3固科萃教装含
54离心机大十等
5.5pH计：测量粘度+0,02pH中证5.8施满泥合器
5.7减教缔汉
5.8班离心管，案因氟烯
6试样制备与保存
股高代表性辞在浆样品：有室湿下辉次态装品部司化片搅定将试样购分感份分别装人样品塑中密封。并标明标记：参作诚验，券…架荐，金制群的操作道程中，应防止摔品活染城发生残必物等量的实化7测定步骤
7.1提取
您取2g试样（精尚创c.e）#！离心管十点1ml水，潮勾静件2mia再加中游全20m，卡旅涡凝合强t以2uccmu感omm离心1uin,过滤移股0.0m消液，加10m）.磷酸热级冲溶演（4择7.2净化
将溶液转移率（周取小中（！礼3m率醇水溶液（.6依次洗涤浓缩，沈漆液进阅相器取小栏，太流液拖！小：.…中掌流脱，整制流惠1m/min2/min收集全部洗照液小cml离心管中，点这个、以：茶浴下减作浓缩至近平，用1.0ml中序-求（1.体积比）器解戏治，部约，游液过（.1，品以滚销色谱瓶语/质谱仪测处7.3测
7.3.！液色请·串联质谱条件
）色谱杜社，1mm为径：5减期消者：5）流动利梯游脱序品英1：
ht
,0. 4 ml./miy:
样串：
离宁源：电露离下源：
扫猫：正肉子烟描
SN/T2576--2010
0.5必甲骏水液/元
检测方式：鑫区应监测：
）等化气服（凯）气解力成流速（GS）向为商纯氮气或H他合适体，议用前应调节名气体流微以及尚子源滑座（小M）倪质谱灵敏度达到检测要求，详细参考条伴效监测离字对（m/餐师图案：
7.3.2高液相色谱-鼠联质增测元根据试样中被测样滋的舍吊，选空激质适的混台基随标雅落液，待测物的响成值成在仪器检测的线性消用内：对混合基质标雅溶液样滴丝康然准证祥测定。在！速倒鸿条件下林可等案、氧称微家吡利需素能参考代留时阅分约光79.？m和9.2mi，标准济液的选择性离流图象见附录3事图3、1，
，筹性测察
按照连条件测实品动滑食心标液如果检测的就景免谱峰保留时混合基游标准1作液微，充许偏器小平5添、效产对的利刘·虚与激度制当耀合整质标准作滋的相对度：致：社对丰度偏关不超过公？的规放，则司判断评品中在和应的被测物家快循舒典中计富魔的最大允许根离工卡度，
金许内对编总案
73.4空自试验
除不加试伴均接「述模法银
结果计算和表述
用货语数据处理机膜接式：贸轩中裤可快腾发药物的残留含量，计算结果带扭除空值：.( 1)
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53/T 2576.-2010bzxz.net
武小：
，一战栏车性安然的，自了微宝年g一基质标准溶液山林时频安美控流，单位为约改客习（/）；栏没展终宗突体限，单位为之升元！股然华液代表的减样防：
9方法的测定低限(00)和国收率
9.1测定低限
补可悦胺炎的物的线商量池低限为三/g9.2博收率
回收率第实验数据（在全同系划浓主：儿支。表林可按类药物添加回收游海圈（%）北合物
样可徐事
华刻索
深州依度
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叫收率
80, 8-181. 2
78. 1-..192. 6
70. 01--103. 0
77. 8-10.0
73. ---93.7
77. 2.-12.4
79..- 1..
73, 5 -. 101,
深料圳树泵）
4000心得/：#统酷离干源新份1
AII4NM客统喷器离考系：
顺需电压：4V
签信气Rh)：89.6 6a4?
re),1s6 16s 2u?? *:
编（Gs23.0.2：k4a）
离了源源度（M10
SV/T 2576--2010
定性离了对完员离博拍能健及室出凹压P见表A1袭A.1
深将素
京林市家茶
利像素
定性离管离华对谢线翻最碰擦家出口电服性案了对
407.226, 3
2..:212. 1
76.03?8.2
1+2:112. 1.
.1.2/383
该离了对为是过离「戏
设撞气能敏(C
1：非商业性所录A所划效品保家效的效列筑验的仪宠少仅是义#金考中沙及容业的及乳实学国的仪肾。http：
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SW/T 2576--2010
：0-1
资性录
林明胶狐药吻选择性离严流图
深林川海素
125. 4/378.2
e2aa.2多源区2
0435 16221113.1 382031734783:.n1.5
氮标海药
425.19/126.1
此刘特票
412/363.1
此利能
A11.2/112.1
a R h o e
1GhIN 12 3.01 2.J1
样得察
407. 2/9.4
5.2/126. 3
林可需素，氧殊问素，北和离案（5，的标准品的选择性离了流图图胜. 1
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SN/r 2576-2010
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Determination f lirwnarniales residues irroyal jelly for impoort anl exrort--Lo-Ms/MsSicope
:This siandard spenifies the miethcd of sample preparation and determinarion of insosamidas residuesin ioyal jellyforimportand expcrt by Lc-Ms/Ms.This stariderd is applicable to the tetorrrinrition of rosidues of linconycin.clincamysin anr pirlimycinn royal feliy.
2Nornmative rererences
e foll:wring rormative docunsarits comiaif swsn: which, thrcugh referance in this tex..cunstituts provisions of this profess!ona atandira. For dateu refererces, subseguent arnendrrnrtsso,c: revisions of,ary of these publicotions rio not apply. Howevef.parties to agreerrents based inthis Pretesional standard are oncouraged tr2 investigate the possibility of apalying the rmost reronleditions ol the normative documents indicatrd below,Fcr undated raferences,the latesi erditico oftharomstive cocumentrefeiredtoappliex.B/ 6682Waterfar analyticai laboratoiy use---Spruification and test rnethodsPrineiple
Methanol :s used to precioitate pisrein.The :tin Supernalarit is diluteci with phosphate hffersolution.The solution is eleaned up wiih Car.idge.h:rewiduasarn deterrmineni by LCMs/Msarni qurnlifiert by exterrai stariard rrsthri.4Heagarts ard inaterials
Uiriless otherwise specified. all regenes tigad shhil kn aralytical grdn, \water is the first grede?water prescribed by GB/t b682.4. +Acotonitrile:HP!.C: gradh.8
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a.Esdiur hyriroxirin
/T 2576--2010
t, D. incl/t. Sarinrm tryeiroxine sirnsr .uigr a s aitn ydreide into 1 t. yalhurnetric tinsk.ilwndituirtnLwihwater
a.t Mnthrnl sr-luicrMetponot water ( + V/y)t. 2hsrhate buffer snlltin: bisscye . E g srdiin ciiyarugen phghate,d:ssolyeat im geio milwra.srvarjust pl . s.0 with o. + rrus/i xtunl mydrvida sotitn awd dilene to \ L with walert.Lirirycintyerrahie:rnilytrare :tenoard rAx No.RsH n-7.CisH..Nu.SxHi,Purityoo. e%. clinarnycin hyerwtileride rCAs : 21te2 : t, u :4n CINet,ssHCI), Puhity s4. 5%.Firlirriystn hytra.ehict co (A3 te:79548-73.5.. y tM sxlkin uriry:ee, 4%.c aiareird stesk solinnritAecumiely we g an acleuate amoun: of eaeh standed (4. B)(aecuratele o, 1 g,rlis:cive in mthearwtl roprtlv. Nr ywtatin f chtin ai is ton ga/nh as the staaneot selution sheread J.a C. Try ar: ch: p r iss morrrs.2. ln Biank sclutin of tiarrpk: Acrxorclirne ts sectieon ?. blank suleticn is pegparerd vwith royal jealywril-tul lncoanide.
, 1rtaisration ctv :tcart woiri n oirier:Aaeg to the, rogirerirrt,dilute th tanduretatrr:k selutis ir: 2 rni/rnl.. ts ng/rih. rignl, tsti p/ol.anrd l? 3g/mnl., mix landard workingiuii:n witi hlah aehtin at samule (d. 1 keir:o ing. it is sames uss 2 g/kg.5 pa/ka lo rg/kes.Fa p/hy and sn pu/kg linaannidas in sarrple.A. 1Ca sualid phinee axtraraticnt tspp wa uy: : sor rng, s mur taailvalent. It sheuld becxndiaianod with s l. nietl n.lrwr.s i r watat.. sMartrm Fi.ler:b. ah: um., rgnt. r:Agtaras art argt:t:airear
t.1Lejnd hrantaphyiid.rn mee rrlryowgulpprd writh electraapray ion tourceh 2Aralytkcal balanric:aruratv:o, try t: ! o. !l sS Elid prnsin erroetin vaeulur rrthtt
SN/T25/6..2010
. 4Certrifuge:6 ono r/min.
5.5pli neter accuracy 0.Q2pil5. 6Werex mixer.
Rotsry vaauum evaporator
t.xCentrifuge tube:Polytetrafhuaroci:ivlnnie.so !.SarnplepreparationandstcrageRoyal jelly is ahout 500 . Tne sariple in, rrisltee ider rwm tomguratire. Keep the prepared samg:leirto two cample boliles,seal and label, Thc !rst ieimpls saerad at rom temperure.\he rast semplo is slored in te rcfrigcialer. i: Fie xiw of sample preparation, rexaut'cshu:l bg Taken to avoid cantaminaticn or Jny facrs,witiel:nay cause the change of residue coner.? Procedure
7. 1 Fxtrastien
Weigh en 2 a test sampie (acrurelt 1o 0. 1 g? irie: st ml rentrifuge tufe. Acded 10 ml warer.mixif. Wait for 2 min. Addl rc 2 rnl. ith tiethci'nt Varesx tet? 1 nin umder 2 ooo r/min.centriiuga farTo nin urider a ooo r/min, then fitrate ann! :grh.p ro, \ nl. sineinetan layer inte a nenrainer. Addt mt. phosphate buffe\ solution t4 7).rnix .2.2 Gleanup
Tranafer the above selution into rartcae t+ .!),tiscard the eluate. The flask anad cariridge isrir:sed with 5 ml water, follower! by ts rnt rf ror:rharks! sinluninn ta. n),d:acad the eluale. Fhetartridge is dried under yacluun tn \dryness\ Fi!lr the carridge wih rnt matharol, flow reteml/min2 rnl/min,The aluate is evarxrate t nearly dyress kncer vaculm inawarsr batnbaicwr o c. Ihe residues are: reccnstitnrcrt in 4. t nil. nethancl-weter (1 + 1, V/v), mix it. hestlutiiisgassed through O.45min fire:Thatilrrateiattariy for IC-Ms/Ms determinatisn.2.3neteminstion
Le-Ms/Msorgratingcoiticans
a)Lc columin:Cs colurnn.i50 mrn x 4. 6 irm t. t.3 atm .or aguivaleast:10
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