食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
2期
421-426
,共6页
陶保华%储小军%赖世云%胡银洲%任一平*
陶保華%儲小軍%賴世雲%鬍銀洲%任一平*
도보화%저소군%뢰세운%호은주%임일평*
香兰素%乙基香兰素%MAX SPE 净化%超高压液相色谱法%同位素稀释液质联用法
香蘭素%乙基香蘭素%MAX SPE 淨化%超高壓液相色譜法%同位素稀釋液質聯用法
향란소%을기향란소%MAX SPE 정화%초고압액상색보법%동위소희석액질련용법
vanillin%ethyl vanillin%MAX SPE%ultra pressure liquid chromatography-ultraviolet spec-trometer%ultra pressure liquid chromatography-mass spectrometry/mass spectrometry
目的建立婴幼儿配方粉中香兰素、乙基香兰素的液相色谱法和同位素稀释液相色谱质谱联用两种测定方法.方法液相色谱法:样品经乙酸锌沉淀蛋白、Oasis MAX SPE 柱净化, HSS T3色谱柱分离后,在279 nm 波长处进行检测,外标法定量.同位素稀释液质联用法:样品采用乙腈沉淀蛋白稀释净化后,采用Waters BEH C18柱分离,在质谱检测器多反应监测(UPLC-MS/MS)模式下,用同位素稀释液质联用法进行检测.结果液相色谱法:香兰素、乙基香兰素的定量下限(LOQ)均为0.1 mg/kg.香兰素的方法回收率为88%~90.8%,相对标准偏差(RSD)小于5.2%;乙基香兰素的方法回收率为84%~93.3%, RSD 小于6.2%.同位素稀释液质联用法香兰素、乙基香兰素的 LOQ 分别为香兰素1、0.5 mg/kg.香兰素、乙基香兰素的方法回收率分别为82.1%~91.2%、90.2%~97.6%, RSD 分别小于6.1%、5.8%.结论本文建立的两种方法对同一样品的检测结果一致,为婴幼儿配方粉中香兰素、乙基香兰素的定量检测提供了较为理想的方法.
目的建立嬰幼兒配方粉中香蘭素、乙基香蘭素的液相色譜法和同位素稀釋液相色譜質譜聯用兩種測定方法.方法液相色譜法:樣品經乙痠鋅沉澱蛋白、Oasis MAX SPE 柱淨化, HSS T3色譜柱分離後,在279 nm 波長處進行檢測,外標法定量.同位素稀釋液質聯用法:樣品採用乙腈沉澱蛋白稀釋淨化後,採用Waters BEH C18柱分離,在質譜檢測器多反應鑑測(UPLC-MS/MS)模式下,用同位素稀釋液質聯用法進行檢測.結果液相色譜法:香蘭素、乙基香蘭素的定量下限(LOQ)均為0.1 mg/kg.香蘭素的方法迴收率為88%~90.8%,相對標準偏差(RSD)小于5.2%;乙基香蘭素的方法迴收率為84%~93.3%, RSD 小于6.2%.同位素稀釋液質聯用法香蘭素、乙基香蘭素的 LOQ 分彆為香蘭素1、0.5 mg/kg.香蘭素、乙基香蘭素的方法迴收率分彆為82.1%~91.2%、90.2%~97.6%, RSD 分彆小于6.1%、5.8%.結論本文建立的兩種方法對同一樣品的檢測結果一緻,為嬰幼兒配方粉中香蘭素、乙基香蘭素的定量檢測提供瞭較為理想的方法.
목적건립영유인배방분중향란소、을기향란소적액상색보법화동위소희석액상색보질보련용량충측정방법.방법액상색보법:양품경을산자침정단백、Oasis MAX SPE 주정화, HSS T3색보주분리후,재279 nm 파장처진행검측,외표법정량.동위소희석액질련용법:양품채용을정침정단백희석정화후,채용Waters BEH C18주분리,재질보검측기다반응감측(UPLC-MS/MS)모식하,용동위소희석액질련용법진행검측.결과액상색보법:향란소、을기향란소적정량하한(LOQ)균위0.1 mg/kg.향란소적방법회수솔위88%~90.8%,상대표준편차(RSD)소우5.2%;을기향란소적방법회수솔위84%~93.3%, RSD 소우6.2%.동위소희석액질련용법향란소、을기향란소적 LOQ 분별위향란소1、0.5 mg/kg.향란소、을기향란소적방법회수솔분별위82.1%~91.2%、90.2%~97.6%, RSD 분별소우6.1%、5.8%.결론본문건립적량충방법대동일양품적검측결과일치,위영유인배방분중향란소、을기향란소적정량검측제공료교위이상적방법.
@@@@Objective To establish quantitative methods of vanillin and ethyl vanillin in infant formulas by a ultra pressure liquid chromatography-ultraviolet spectrometer (UPLC-UV) and a ultra pressure liquid chromatography-mass spectrometry/mass spectrometry (UPLC-MS/MS). Methods In the UPLC-UV method, samples were purified and concentrated by Oasis MAX solid-phase extraction (SPE) cartridges after protein precipitation with zinc acetate. The vanzillin and ethyl vanillin elution were separated by an HSS T3 column, and detected by the UV detector at a wavelength of 279 nm. In the UPLC-MS/MS method, the protein was pre-cipitated by acetonitrile. The supernatant were separated by a Waters BEH C18 column and quantified by iso-tope dilution liquid chromatography combined with mass spectrometry under multiple reaction monitoring (MRM) mode. Results LOQ of vanillin and ethyl vanillin were 0.1 mg/kg, as well as the overall spiked re-coveries were 88%~90.8% (RSD<5.3%) for vanillin and 90.2%~97.6% (RSD<6.5%) for ethyl vanillin in UPLC-UV method. In UPLC-MS/MS method, LOQ of vanillin and ethyl vanillin were 1 mg/kg and 0.5 mg/kg, and the overall spiked recoveries were 82.1%~91.2% (RSD<6.1% ) for vanillin and 90.2%~97.6% (RSD<5.8%) for ethyl vanillin. Conclusion As the similar performances including good repeatability and high sensitivity, UPLC-UV and UPLC-MS/MS can be used as a routine method for the determination of e vanillin and ethyl va-nillin in infant formulas.
