银离子固相萃取-程序升温大体积进样-气相色谱法定量分析市售巧克力中的饱和烷烃矿物油

建立了银渍硅胶固相萃取柱离线（Ag-SPE)净化，程序升温进样-气相色谱-氢火焰离子化检测器(PTV-GC-FID)定量分析巧克力中饱和烷烃矿物油（MOSH)的方法。以正己烷浸泡提取巧克力中的MOSH，离心后取1mL上清液，过0.3%Ag渍硅胶SPE柱净化，氮吹浓缩，定容至0.2mL，注人GC分析；GC的进样口程序升温过程:初始温度45益，保持1min(分流比200颐1)，以250益/min升温至360益（分流阀关闭2min)，并保持27min(分流比100:1);进样量40滋L;柱温箱升温程序为：35益保持3min，以25益/min升温至350益，以5益/min升温至370益，保持10min...

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Bibliographic Details
Published in分析化学 Vol. 45; no. 4; pp. 514 - 520
Main Author 李冰宁;刘玲玲;张贞霞;武彦文
Format Journal Article
LanguageChinese
Published 北京市理化分析测试中心,北京市食品安全测试工程技术研究中心,北京市科学技术研究院分析测试技术重点实验室,北京 100089%西安通信学院,西安,710106 2017
Subjects
巧克力;矿物油污染;饱和烷烃;固相萃取;气相色谱法;氢火焰离子化检测器
气相色谱法
Solid phase extraction
Gas chromatography
Mineral oil contamination
Hydrogen flame ionization detector
固相萃取
Chocolate
Saturated hydrocarbons
氢火焰离子化检测器
饱和烷烃
巧克力
矿物油污染
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Summary:建立了银渍硅胶固相萃取柱离线（Ag-SPE)净化，程序升温进样-气相色谱-氢火焰离子化检测器(PTV-GC-FID)定量分析巧克力中饱和烷烃矿物油（MOSH)的方法。以正己烷浸泡提取巧克力中的MOSH，离心后取1mL上清液，过0.3%Ag渍硅胶SPE柱净化，氮吹浓缩，定容至0.2mL，注人GC分析；GC的进样口程序升温过程:初始温度45益，保持1min(分流比200颐1)，以250益/min升温至360益（分流阀关闭2min)，并保持27min(分流比100:1);进样量40滋L;柱温箱升温程序为：35益保持3min，以25益/min升温至350益，以5益/min升温至370益，保持10min，载气为髙纯氮气，流速1.3mL/min(压力60kPa);FID温度为380益。结果表明，本方法的MOSH定量限为0.5mg/kg，加标回收率为84.9%~108.6%，相对标准偏差(RSD)为0.2%~1.5%。运用本方法对25个市售巧克力样品中的MOSH含量进行了测定，3个样品未检出，其余22个样品中MOSH含量为1.09~8.15mg/kg(其中C16~C35的含量为0.56~4.43mg/kg)，有3个样品含量髙于5.00mg/kg，为严重污染样品。本方法操作简便，检出限低，适用于巧克力中MOSH的定量测定。
Bibliography:An offline silver-impregnated silica gel solid-phase extraction(Ag-SPE)approach combined with aprogrammed temperature vaporization-gas chromatography-flame ionization detector(PTV-GC-FID)wasproposed for routine analysis of mineral oil saturated hydrocarbons(MOSH)in chocolates.The MOSH inchocolates were extracted by n-hexane and1mL of extract was purified by offline Ag-SPE column.The SPEcolumns packed with0.3%Ag-activated silica gel were used to separate MOSH from triglycerides and olefinsin chocolates.The eluent of MOSH fraction was only5mL and then concentrated to0.2mL through nitrogenblowing with little evaporation loss.The PTV parameters were as follows:the initial temperature was set at45益and held for1min(split ratio was200颐1),then warmed up to360益at linear gradient of250益min1and held for27min(split valve was closed for2min followed by split ratio of100颐1).The GC injectionvolume was40滋L.The GC column was heated from35益(3min)to350益at25益/min,and then raised to370益(10min)at5益/min.The flow rate of the carrier
ISSN:0253-3820
DOI:10.11895/j.issn.0253-3820.160828