高效液相色谱-离子阱质谱法快速筛查改善睡眠类保健食品中非法添加的24种镇静催眠药.pdf

《高效液相色谱-离子阱质谱法快速筛查改善睡眠类保健食品中非法添加的24种镇静催眠药.pdf》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。

1、2015年3月色谱1青Vo1．33No．3March20l5ChineseJournalofChromatography256～266研究论文D0I：1()．3724／SP．J．1I23．2()I4．1t()()l摘要：建立r『岛效液十『1色谱一离子阱质谱(HPLC—ITMS)M【J1『测定改善睡眠炎健tjfIf法添的24种锁催眠药的快速筛办‘法。样品经甲醇超声提取20min，经0．45m滤膜过滤进仃HPLC—ITMS分析榆洲永川PhenomenexLunaC18色谱柱分离，流动卡IlA为0．05％(v／v)甲酸水溶液，流功十lJB为甲醉一乙腑(15：25，

2、v／v)溶液，等度洗脱；采川电喷劈离子(ESI)源及l饥离f}JJ换幞』℃，}1描MS～MS、级质渚，利川24种约物的MS／MS(MS)和MS／MS／MS(MS)质谱对样品进仃定筛务24种镇静催眠约I^-定线什范【纠内线性父系，flI关系数(r)均人j：0．999，榆出限在4．0～446．6~tg／L之问，3个添加水平n勺【¨iI收为88．6％～Il0．3％，十ll埘准偏蓐(RSD)0．8％～9．8％之。27批样品纶筛发现彳丁I8批样II检m褪索该方法快速、敏、处法，町用于保健食t^lf1法添加镇静催眠类药；^的快速筛关键词：舟效液十¨色一离予阱质潜；镇静叭

3、约tI一＼；保健食品；快速筛中图分类号：0658文献标识码：A文章编号：1000—87l3(2015)03—0256—11Abstract：Afastscreeningmethodwasestablishedforthesimultaneousdeterminationof24sedativehypnoticsillegallyaddedinimprovingsleephealthfoodsbyhighperformanceliquidchromatography—iontrapmassspectrometry(HPLC—ITMS)．Themethodwas

4、basedontheson—icationassistedextractionoftheimprovingsleephealthfoodsamplesusingmethano1．Theex—tractwasthenfiltratedwith0．45p,mfiltermembraneandthefiltratewasseparatedonaPhe—nomenexLunaCl8columnwithisocraticelutionataflowrateof0．3mL／min．Abinarymobilephasewas0．05％(v／v)formicacid(sol

5、ventA)一methano1／acetonitrile(15：25，v／v，solventB)．Theelectrosprayionization(ESI)sourceinpositiveionmodeornegativeionmodewasusedtoscanMS一MSspectraforthe24sedativehypnotics．TheMSandMS’spectrawereusedforqualitativeanalysisofsamples．Thecalibrationgraphswerelinearintheirconcentra—tionran

6、geswiththecorrelationcoeficients(r!)morethan0．999．Thelimitsofdetection(LODs)were4．0—446．6&g／L．Therecoveriesforallthedrugsintheimprovingsleephealthfoodswere88．6％一l10．3％withtherelativestandarddeviationsnomorethan9．8％atthreespikedlevels．Twenty—sevenbatchesoftheimprovingsleephealthfood

7、sweretested．Melatoninwasfoundineighteenbatches．Themethodisfast，specific，sensitive，easyandsuitableforfastscreeningof24sedativehypnoticsillegallyaddedinimprovingsleephealthfoods．Keywords：highperformanceliquidchromatography—iontrapmassspectrometry(HPI—C—ITMS)；sedativehypnotics；healthf

8、oods；fastscreening通讯联系人rre