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江苏 气相色谱仪检测动植物油脂、脂肪酸甲酯含量(气相色谱法)

来宝网 2012/4/12点击3082次

<p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’">本方法引用标准及应用范围</span><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; text-indent: 15.75pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">本方法完全满足<font face="Times New Roman">GB/T17377-2008</font><font face="宋体">《动植物油脂&nbsp;&nbsp;脂肪酸甲酯的气相色谱分析》以及</font><font face="Times New Roman">GB/T17376-2008</font><font face="宋体">《动植物油脂&nbsp;&nbsp;脂肪酸甲酯制备》中的规定。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’">本方法可以检测下列各种植物油品种</span><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; text-indent: 15.75pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">1<font face="宋体">)豆油,主要脂肪酸组成是亚油酸</font><font face="Times New Roman">50%</font><font face="宋体">-</font><font face="Times New Roman">55%</font><font face="宋体">,油酸</font><font face="Times New Roman">22%</font><font face="宋体">-</font><font face="Times New Roman">25%</font><font face="宋体">,棕榈酸</font><font face="Times New Roman">10%</font><font face="宋体">-</font><font face="Times New Roman">12%</font><font face="宋体">,亚麻酸</font><font face="Times New Roman">7%</font><font face="宋体">-</font><font face="Times New Roman">9%</font><font face="宋体">。亚油酸和&alpha;-亚麻酸是两种人体必需的脂肪酸。精炼豆油中维生素</font><font face="Times New Roman">E</font><font face="宋体">的含量为</font><font face="Times New Roman">60</font><font face="宋体">-</font><font face="Times New Roman">110mg/100g</font><font face="宋体">。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;&nbsp;2<font face="宋体">)菜籽油,其脂肪酸的组成受气候、品种等的影响较大。菜籽油中含有较多可能对健康不利的芥酸,其主要脂肪酸组成是亚油酸</font><font face="Times New Roman">10%</font><font face="宋体">-</font><font face="Times New Roman">20%</font><font face="宋体">,油酸</font><font face="Times New Roman">10%</font><font face="宋体">-</font><font face="Times New Roman">35%</font><font face="宋体">,棕榈酸</font><font face="Times New Roman">2%</font><font face="宋体">-</font><font face="Times New Roman">5%</font><font face="宋体">,亚麻酸</font><font face="Times New Roman">5%</font><font face="宋体">-</font><font face="Times New Roman">15%</font><font face="宋体">,芥酸</font><font face="Times New Roman">25%</font><font face="宋体">-</font><font face="Times New Roman">55%</font><font face="宋体">,花生四烯酸</font><font face="Times New Roman">7%</font><font face="宋体">-</font><font face="Times New Roman">14%</font><font face="宋体">。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;&nbsp;&nbsp;3<font face="宋体">)花生油,具有独特的花生气味和风味,可直接用于制造起酥油、人造奶油、蛋黄酱,也是良好的煎炸油。花生油的脂肪酸组成比较独特,含有</font><font face="Times New Roman">6%</font><font face="宋体">-</font><font face="Times New Roman">7%</font><font face="宋体">的长链脂肪酸,因此,花生油具有良好的氧化稳定性。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;&nbsp;&nbsp;4<font face="宋体">)玉米油,又称为玉米胚芽油、粟米油,主要脂肪酸组成是亚油酸</font><font face="Times New Roman">55%</font><font face="宋体">-</font><font face="Times New Roman">60%</font><font face="宋体">,油酸</font><font face="Times New Roman">25%</font><font face="宋体">-</font><font face="Times New Roman">30%</font><font face="宋体">,棕榈酸</font><font face="Times New Roman">10%</font><font face="宋体">-</font><font face="Times New Roman">12%</font><font face="宋体">,亚麻酸</font><font face="Times New Roman">2%</font><font face="宋体">以下。玉米油含亚油酸高,其降血清胆固醇的效能优于其他油脂。又由于玉米油富含维生素</font><font face="Times New Roman">E</font><font face="宋体">,所以,其氧化稳定性也较好。</font><font face="Times New Roman">&nbsp;</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;&nbsp;&nbsp;5<font face="宋体">)葵花籽油,是为数不多的高亚油酸油脂之一,故有人将它与玉米油列为&ldquo;健康保健油脂&rdquo;。其主要脂肪酸组成是亚油酸</font><font face="Times New Roman">65%</font><font face="宋体">-</font><font face="Times New Roman">78%</font><font face="宋体">,油酸</font><font face="Times New Roman">14%</font><font face="宋体">-</font><font face="Times New Roman">17%</font><font face="宋体">,棕榈酸</font><font face="Times New Roman">6%</font><font face="宋体">-</font><font face="Times New Roman">8%</font><font face="宋体">,硬脂酸</font><font face="Times New Roman">2%</font><font face="宋体">-</font><font face="Times New Roman">3%</font><font face="宋体">,维生素</font><font face="Times New Roman">E</font><font face="宋体">的含量为</font><font face="Times New Roman">100mg/100g</font><font face="宋体">,还含有绿原酸,其氧化稳定性好,但它不宜单独用于煎炸食品。</font><font face="Times New Roman">&nbsp;</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;&nbsp;6<font face="宋体">)</font><font face="Times New Roman">&nbsp;</font><font face="宋体">橄榄油,是从油橄榄鲜果中直接压榨出来的果汁,分离掉其中的水分后取得。单不饱和脂肪酸含量高达</font><font face="Times New Roman">80%</font><font face="宋体">以上,必需脂肪酸亚油酸与亚麻酸的比例为</font><font face="Times New Roman">1</font><font face="宋体">:</font><font face="Times New Roman">4</font><font face="宋体">,正好符合人体对摄入脂肪的标准,对人体健康尤其是心脏健康有益。世界卫生组织调查表明,以橄榄油为首选食用油的希腊,心血管系统和癌症发病率极低。</font><font face="Times New Roman">&nbsp;</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><br /> </span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">&nbsp;&nbsp;7<font face="宋体">)</font><font face="Times New Roman">&nbsp;&nbsp;</font><font face="宋体">茶油,是利用油茶的种子榨制的一种优质食用油。茶油含有丰富的维生素</font><font face="Times New Roman">E</font><font face="宋体">、</font><font face="Times New Roman">D</font><font face="宋体">、</font><font face="Times New Roman">K</font><font face="宋体">和-胡萝卜素,不饱和脂肪酸含量高达</font><font face="Times New Roman">85%</font><font face="宋体">-</font><font face="Times New Roman">97%</font><font face="宋体">,比橄榄油的含量还要高,茶油还含有茶多酚和茶皂甙,对降低胆固醇和抗癌有明显的功效。二、二、实验原理</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">本实验甲酯化方法采用国标<font face="Times New Roman">GB/T&nbsp;17376-2008</font><font face="宋体">,甘油酯皂化后,释出的脂肪酸进行酯化,萃取得到脂肪酸甲酯用于气相色谱分析。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">样品中的脂肪酸经过适当的前处理(甲酯化)后,进样,样品在汽化室被汽化,在一定的温度下,汽化的样品随载气通过色谱柱,由于样品中组分与固定相间相互用的强弱不同而被逐一分离,分离后的组分,到达检测器时经检测口的相应处理,产生可检测的信号。根据色谱峰的保留时间定性,归一法确定不同脂肪酸的百分含量。</span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’">仪器及试剂配置</span><span style="font-family: ’宋体’; font-size: 10.5pt; font-weight: bold; mso-spacerun: ’yes’"><o:p></o:p></span></p> <p> <table style="padding-bottom: 0pt; padding-left: 5.4pt; padding-right: 5.4pt; border-collapse: collapse; margin-left: -3.6pt; padding-top: 0pt; mso-table-layout-alt: fixed"> <tbody> <tr style="height: 7.25pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: rgb(0,0,0) 0.5pt solid; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">检测项目</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: rgb(0,0,0) 0.5pt solid; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">植物油中脂肪酸的测定</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> <tr style="height: 3.5pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">色谱仪器型号</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">GC5890<font face="宋体">型色谱仪&nbsp;&nbsp;&nbsp;配有</font><font face="Times New Roman">FID</font><font face="宋体">检测器</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> <tr style="height: 3.5pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">毛细管色谱柱</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">PEG-20M30*0.32*0.5<font face="宋体">专用柱</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> <tr style="height: 3.5pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">色谱工作站<font face="Times New Roman">N2000</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">(电脑<font face="Times New Roman">1</font><font face="宋体">台自备)</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> <tr style="height: 3.5pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: rgb(255,255,255) 31.875pt; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 31.8750pt none rgb(255,255,255)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">氮氢空发生器</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: rgb(255,255,255) 31.875pt; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 31.8750pt none rgb(255,255,255)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">HGT300E&nbsp;1<font face="宋体">台或高纯氮、氢气、空气钢瓶各一瓶</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> <tr style="height: 23.25pt"> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: rgb(0,0,0) 0.5pt solid; padding-bottom: 0pt; padding-left: 5.4pt; width: 144pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: 0.5000pt solid rgb(0,0,0); mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="192"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">其它仪器</span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> <td style="border-bottom: rgb(0,0,0) 0.5pt solid; border-left: medium none; padding-bottom: 0pt; padding-left: 5.4pt; width: 270pt; padding-right: 5.4pt; border-top: medium none; border-right: rgb(0,0,0) 0.5pt solid; padding-top: 0pt; mso-border-bottom-alt: 0.5000pt solid rgb(0,0,0); mso-border-left-alt: none; mso-border-right-alt: 0.5000pt solid rgb(0,0,0); mso-border-top-alt: 0.5000pt solid rgb(0,0,0)" valign="top" width="360"> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">1<font face="宋体">.恒温水浴锅</font><font face="Times New Roman">2</font><font face="宋体">.移液管</font><font face="Times New Roman">3</font><font face="宋体">.胶头滴管</font><font face="Times New Roman">4</font><font face="宋体">.小圆底烧瓶</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> <p style="text-align: center; margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">5<font face="宋体">.冷凝管</font><font face="Times New Roman">6.&nbsp;</font><font face="宋体">样品瓶</font></span><span style="font-family: ’宋体’; font-size: 10.5pt"><o:p></o:p></span></p> </td> </tr> </tbody> </table> </p> <p style="margin-top: 0pt; margin-bottom: 0pt" class="p0"><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’">试剂:<font face="Times New Roman">.</font><font face="宋体">石油醚、乙醚、氢氧化钾、甲醇均为</font><font face="Times New Roman">AR</font><font face="宋体">级。</font></span><span style="font-family: ’宋体’; font-size: 10.5pt; mso-spacerun: ’yes’"><o:p></o:p></span></p> <!--EndFragment-->

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