固相萃取-超高效液相色谱-串联质谱法同时测定饲料中的3种雌激素.pdf

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1、20l4q-：llJJ色谱Vo1．32NO．IlNovember20l4ChineseJournalofChromatographyl209～l2l3研究论文DOI：10．3724／SP．J．1l23．20I4．07039摘要：建r【占1相苷取一超离效液相色潸一联质潜(SPE—UPLC—MS／MS)Mfllf测定州料(预混合、配合和浓缩州料)llI3种雌激素(1一雌二醇、水l}1酸雌孵和戊酸雌二)的检测办法饲料样品乙腈提取，HeaionC。固取净化后，川ACQUITYUPLCBEHC．色谱(501]lnlx2．1mm，1．7m)分离，乙腑和O．1％氨水溶液作为流动卡H逊仃梯度洗

2、脱．多反监测(MRM)模式愉测，标法定结明，1一雌二醇卡¨戊酸雌l一醇在l0～200p,g／L、⋯酸雌5～200g／L范崮内j仃良r线一H-，卡¨父系数(?’)≥0．99617卢一雌_I醇、苯⋯酸雌一醇和戊陵雌二雕的愉fIj分圳为7、5平¨7p．g／kg样的j均JJl1怀⋯收牢为96．5％～102．0％该法处操作简便、分析速度伙、榆fff低、准确度商，可ffJj饲料If-3种雌激索的川『flf检测关键词：川十H萃圾；趟高效液卡¨色谱一f”联质谱；】7一雌一雕；苯qI酸雌_二醇；酸雌醇；饲料中图分类号：O658文献标识码：A文章编号：l000—8713(20l4)l1一l209—

3、05Abstract：Amethodwasdevelopedforthesimultaneousdeterminationofthreeestrogens(17一estradiol，estradiolbenzoate，estradiolvalerate)infeedbysolidphaseextraction—ultraperformanceliquidchromatography—tandemmassspectrometry(SPE—UPLC—MS／MS)．Afterthesamplewasextractedbyacetonitrileandcleaned—uponaHeai

4、onCI8solidphaseextraction(SPE)column，thethreeestrogenswereseparatedbyanACQUITYUPLCBEHCI8column(50mmx2．111／ITI，1．7m)withgradientelutionusingacetonitrileand0．1％ammoniasolutionasmobilephasesandfinallyconfirmedandquantifiedinmultiplereactionmonitoring(MRM)mode．Theinternalstandardcalibrationcurve

5、swereusedforthequantification．Theresultsshowedthatalltheestrogensweredeterminedwithexcellentlinearrelationshipsfroml0p~g／Lto200p~g／Lforl7卢一estradiolandestradiolvalerate，andfrom5g／Lto200g／Lforestradiolbenzoate．Thecorrelationcoeficients(7’)ofthethreeestrogenswerenotlowerthan0．996．Thelimitsofde

6、tectionfor17B—estradio1．estradiolbenzoateandestradiolvaleratewere7~g／kg．5ptg／kgand7~g／kg．respectively．Theaveragerecoverieswere96．5％一l02．0％．Theresultsdemonstratedthatthedevelopedmethodcansimultaneouslydeterminethethreeestro—gensinfeedwithadvantagesofsimplepretreatment，rapidanalysis，lowlimitof

7、detectionandhighaccuracy．}通讯联系人Tel：(028)6509913I，E—mail：xqw66666@I63．COn]．基金项目：四川省科技荩础条件平台建设专项；成都Ji『科技计划项口(12RKYBl74ZF一001)收稿日期：2Ol4—07—23·1210·色谱第32卷Keywords：solidphaseextraction(SPE)；ultraperformanceliquidchromatography—tandemmassspectrometry(UPL