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1、第42卷第3期西北農(nóng)林科技大學學報(自然科學版)Vo1.42No.32014年3月JournalofNorthwestA8LFUniversity(Nat.Sci.Ed.)Mar.2014網(wǎng)絡出版時間:2014—02—2813:13DOI:10.13207/j.cnki.jnwafu.2014.03.020網(wǎng)絡出版地址:http://www.enki.net/kems/doi/10.13207/j.cnki.jnwafu.2014.03.020.html瘋草中苦馬豆素的固相萃取一親水作用色譜檢測李金成,楊國棟,王研,康丹菊
2、,李艷紅,耿果霞,王建華(西北農(nóng)林科技大學動物醫(yī)學院,陜西楊凌712ioo)[摘要]【目的】建立瘋草中苦馬豆素的固相萃取一親水作用色譜分析方法?!痉椒ā恳孕』埂⒚昙?、黃花棘豆、甘肅棘豆、冰III棘豆等5種瘋草為樣品,經(jīng)純乙醇索氏提取和SPE固相萃取柱凈化,采用Watersx—BredgeHILIC色譜柱和蒸發(fā)光散射檢測器,對流動相中的有機溶劑種類及質(zhì)量濃度、緩沖鹽濃度和柱溫等條件進行優(yōu)化,檢測苦馬豆素含量并用質(zhì)譜檢測法進行驗證?!窘Y(jié)果】苦馬豆素與瘋草中的其他成分在異丙醇一2mmol/L乙酸銨(體積比為52:48)流
3、動相條件下可以得到較好地分離;苦馬豆素在1O~100/,g/mL的質(zhì)量濃度與色譜峰面積具有良好的線性關(guān)系(r:0.997),檢出限(LOD)(信噪比一3)為6/,g/mL,定量限(LOQ)(信噪比一10)為20/~g/mL,加標回收率在8O~100?!窘Y(jié)論】建立的固相萃取一親水作用色譜檢測方法簡單、快速、精密度和準確度高,可替代傳統(tǒng)的陽離子交換樹脂凈化一衍生化法用于瘋草中苦馬豆素的測定。[關(guān)鍵詞]固相萃??;親水色譜法;瘋草;苦馬豆素[中圖分類號]$859.87[文獻標志碼]A[文章編號]1671—9387(2014)03—
4、0056—06DeterminationofswainsonineinIocoweedsbyhydrophilicinteractionchromatographycombinedwithsolidphaseextractionLIJin—cheng,YANGGuo—dong,WANGYan,KANGDan-ju,LIYan—hong,GENGGuo—xia,WANGJian—hua(CollegeofVeterinaryMedicine,NorthwestA&FUniversity,Yangling,Shaanxi712
5、100。China)Abstract:[Objective]Thisstudyestablishedahydrophilicinteractionliquidchromatographycombinedwithsolidphaseextractionmethod(SPE—HILIC)forthedeterminationofswainsonineinlocoweeds.[Method]Oxytropisglabra,0.sericopetala,0.ochrocepala,0.kansuensis,andAstragalu
6、sstrictuswerecollectedassamplesoflocoweeds.Thesampleswereextractedwithethylethanol,purifiedwithsolidphaseextractioncolumnandanalyzedbyaWatersX—BredgeHILICcolumn,andthenswainsoninewasdetectedbyevaporativelightscatteringdetector.Theextractionconditionsincludingorgan
7、icsolventsandtheircon—centrations,buffersaltconcentration,andcolumntemperaturewereoptimizedandtheresultswerevalida—tedusingmassspectrometry.[Result]Swainsoninewasseparatedfromothercomponentsinextractsoflo—coweedswithmobilephaseofisopropanol一2mmol/Lammoniumacetate(
8、volumeratiowas52:48).Thecalibrationcurvewaslinearwithintherangeof10—100/~g/mL(r一0.997),thedetectionlimitwas6/~g/mLandthelimitofquantitationwas20/~g/mL.T