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1、20l4q-:llJJ色譜Vo1.32NO.IlNovember20l4ChineseJournalofChromatographyl209~l2l3研究論文DOI:10.3724/SP.J.1l23.20I4.07039摘要:建r【占1相苷取一超離效液相色潸一聯(lián)質(zhì)潛(SPE—UPLC—MS/MS)Mfllf測定州料(預(yù)混合、配合和濃縮州料)llI3種雌激素(1一雌二醇、水l}1酸雌孵和戊酸雌二)的檢測辦法飼料樣品乙腈提取,HeaionC。固取凈化后,川ACQUITYUPLCBEHC.色譜(501]lnlx2.1mm,1.7m)分離,乙腑和O.1%氨水溶液作為流動卡H遜仃梯度洗
2、脫.多反監(jiān)測(MRM)模式愉測,標(biāo)法定結(jié)明,1一雌二醇卡¨戊酸雌l一醇在l0~200p,g/L、?酸雌5~200g/L范崮內(nèi)j仃良r線一H-,卡¨父系數(shù)(?’)≥0.99617盧一雌_I醇、苯?酸雌一醇和戊陵雌二雕的愉fIj分圳為7、5平¨7p.g/kg樣的j均JJl1懷?收牢為96.5%~102.0%該法處操作簡便、分析速度伙、榆fff低、準(zhǔn)確度商,可ffJj飼料If-3種雌激索的川『flf檢測關(guān)鍵詞:川十H萃圾;趟高效液卡¨色譜一f”聯(lián)質(zhì)譜;】7一雌一雕;苯qI酸雌_二醇;酸雌醇;飼料中圖分類號:O658文獻標(biāo)識碼:A文章編號: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盧一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.}通訊聯(lián)系人Tel:(028)6509913I,E—mail:xqw66666@I63.COn].基金項目:四川省科技藎礎(chǔ)條件平臺建設(shè)專項;成都Ji『科技計劃項口(12RKYBl74ZF一001)收稿日期:2Ol4—07—23·1210·色譜第32卷Keywords:solidphaseextraction(SPE);ultraperformanceliquidchromatography—tandemmassspectrometry(UPL