CN103969380A - 一种利用化学计量法定性检测植物油中掺伪油脂的方法 - Google Patents
一种利用化学计量法定性检测植物油中掺伪油脂的方法 Download PDFInfo
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Abstract
本发明公开了一种利用化学计量法定性检测植物油中掺伪油脂的方法,包括如下步骤:气相色谱数据获取,使用判别分析和聚类分析对植物油中所掺入的油脂种类进行鉴别。建立了13个判别分析模型,待侧样品检测省去了与标准植物油图谱比对及脂肪酸含量比对等步骤,直接将其脂肪酸比例代入即可鉴定掺伪植物油种类,可实现米糠油中掺棕榈油、菜籽油、棉籽油、大豆油、茶籽油、花生油的鉴定,检测准确率96%以上。米糠油掺棕榈油、菜籽油、棉籽油、大豆油的聚类分析能鉴别掺伪9%以上的棕榈油、掺伪2%以上的菜籽油、掺伪5%以上的棉籽油、掺伪16%以上的大豆油。
Description
技术领域
本发明涉及一种利用化学计量法快速检测植物油中掺伪油脂的方法,尤其是涉及一种检测米糠油中掺入的棕榈油、棉籽油、大豆油、菜籽油的方法。
背景技术
米糠油是稻谷加工过程中产生的米糠经过压榨或浸提制取的油脂。全球稻谷年产量约为6.38亿,米糠约占稻谷5.2%-7.5%,米糠中脂肪含量约为16%-22%,因此1kg的米糠油约需要100~150kg的稻谷。米糠油生产对设备要求较高,米糠原油含较多的游离脂肪酸对精炼要求高,且米糠极易氧化,因此米糠油成产成本相对较高。国内米糠油的价格比棕榈、菜籽油、棉籽油、大豆油高出不少,由于利润驱使上述油脂常被掺入纯高价食用油或调和油而未在标签中说明。目前对米糠油的掺伪检测极少。
CN103217393A于2013年7月24日公开了一种茶油掺伪的检测方法,建立折光率、碘值、皂化值和油酸含量掺伪检测模型,方法不适合于低级油脂掺入米糠油的情况。
发明内容
本发明旨在克服现有技术的不足,提供一种准确度高、重现性好、快捷便利的利用化学计量法定性检测掺伪油脂的方法。
为了达到上述目的,本发明提供的技术方案为:
所述利用化学计量法定性检测植物油中掺伪油脂的方法包括如下步骤:
(1)采用气相色谱法测定待测植物油中各脂肪酸的含量;该步骤采用的气相色谱法为常规方法,参数为本领域技术人员可调,采用柱室220℃恒温或程序升温法;毛细管色谱柱;外标法、内标法或归一法计算各脂肪酸的含量(均为本领域常规方法);
(2)将待测植物油的脂肪酸含量代入以下13个计算模型中,以下模型所依据的色谱数据来源于129个标准植物油的脂肪酸含量测定值,其中米糠油33种,来源于国内6个稻作区的稻谷,实验室制备而成,棕榈油8种来源于马来西亚,其它植物油国内市售;计算Y1至Y13的数值结果:
Y1=949.821×C10:0+143.946×C14:0+89.515×C16:0+181.532×C16:1+359.968×C17:0+107.006×C18:0+101.592×C18:1+105.504×C18:2+93.738×C18:3+133.945×C20:0+140.364×C20:1+73.022×C22:0+55.167×C22:1-5031.548;
Y2=1438.311×C10:0+139.412×C14:0+91.792×C16:0+185.061×C16:1+361.166×C17:0+111.856×C18:0+100.457×C18:1+103.234×C18:2+94.770×C18:3+131.944×C20:0+138.912×C20:1+77.803×C22:0+55.222×C22:1-5049.374;
Y3=833.672×C10:0+134.870×C14:0+85.436×C16:0+172.626×C16:1+637.630×C17:0+98.978×C1 8:0+96.660×C18:1+98.821×C18:2+93.030×C18:3+144.994×C20:0+144.031×C20:1+66.448×C22:0+61.036×C22:1-4682.546;
Y4=896.353×C10:0+128.253×C14:0+84.320×C16:0+162.165×C16:1+384.505×C17:0+118.244×C18:0+101.018×C18:1+101.485×C18:2+89.035×C18:3+128.214×C20:0+136.708×C20:1+65.445×C22:0+50.248×C22:1-4852.422;
Y5=928.799×C10:0+152.520×C14:0+90.314×C16:0+189.679×C16:1+388.121×C17:0+114.050×C18:0+100.355×C18:1+106.986×C18:2+88.392×C18:3+122.661×C20:0+138.219×C20:1+71.585×C22:0+57.269×C22:1-5088.379;
Y6=910.200×C10:0+139.206×C14:0+89.538×C16:0+179.837×C16:1+377.844×C17:0+110.874×C18:0+101.812×C18:1+105.471×C18:2+91.924×C18:3+123.842×C20:0+145.055×C20:1+128.863×C22:0+52.648×C22:1-5159.902;
Y7=1040.664×C10:0+138.386×C14:0+89.206×C16:0+176.115×C16:1+446.255×C17:0+118.737×C18:0+101.533×C18:1+106.535×C18:2+104.723×C18:3+126.953×C20:0+137.938×C20:1+75.991×C22: 0+54.122×C22:1-5174.614;
Y8=1332.938×C10:0+141.742×C14:0+90.311×C16:0+180.668×C16:1+362.246×C17:0+111.429×C18:0+101.825×C18:1+105.543×C18:2+93.779×C18:3+134.566×C20:0+141.212×C20:1+72.544×C22:0+55.215×C22:1-5089.915;
Y9=900.173×C10:0+138.162×C14:0+87.246×C16:0+175.240×C16:1+487.459×C17:0+102.642×C18:0+99.064×C18:1+101.769×C18:2+94.465×C18:3+143.622×C20:0+147.800×C20:1+68.062×C22:0+56.071×C22:1-4816.328;
Y10=900.399×C10:0+136.828×C14:0+88.591×C16:0+177.154×C16:1+382.924×C17:0+113.400×C18:0+103.289×C18:1+104.908×C18:2+93.751×C18:3+131.177×C20:0+141.241×C20:1+73.050×C22:0+53.048×C22:1-5100.582;
Y11=934.574×C10:0+148.182×C14:0+90.524×C16:0+186.865×C16:1+374.092×C17:0+111.813×C18:0+101.489×C18:1+106.812×C18:2+91.637×C18:3+128.999×C20:0+140.408×C20:1+72.549×C22:0+56.431×C22:1-5107.566;
Y12=918.758×C10:0+140.704×C14:0+90.251×C16:0+181.331×C16:1+373.097×C17:0+112.340×C18:0+102.454×C18:1+106.129×C18:2+93.098×C18:3+135.285×C20:0+145.736×C20:1+99.281×C22:0+53.892×C22:1-5147.272;
Y13=949.965×C10:0+139.427×C14:0+90.171×C16:0+180.058×C16:1+454.214×C17:0+117.458×C18:0+102.039×C18:1+106.534×C18:2+100.227×C18:3+126.549×C20:0+140.273×C20:1+76.189×C22: 0+54.286×C22:1-5154.243;
其中,Y1表示米糠油,Y2表示棕榈油,Y3表示菜籽油,Y4表示茶籽油,Y5表示棉籽油,Y6表示花生油,Y7表示大豆油,Y8表示掺混棕榈油的米糠油,Y9表示掺混菜籽油的米糠油,Y10表示掺混茶籽油的米糠油,Y11表示掺混棉籽油的米糠油,Y12表示掺混花生油的米糠油,Y13表示掺混大豆油的米糠油;
若待测植物油的Y1至Y13中Y1的数值最大,则该植物油为米糠油;若Y2最大,则该植物油为棕榈油;若Y3最大,则该植物油为菜籽油;若Y4最大,则该植物油为茶籽油;若Y5最大,则该植物油为棉籽油;若Y6最大,则该植物油为花生油,若Y7最大,则该植物油为大豆油;若Y8最大,则该植物油为掺混棕榈油的米糠油;若Y9最大,则该植物油为掺混菜籽油的米糠油;若Y10最大,则该植物油为掺混茶籽油的米糠油;若Y11最大,则该植物油为掺混棉籽油的米糠油;若Y12最大,则该植物油为掺混花生油的米糠油;若Y13最大,则该植物油为掺混大豆油的米糠油。
优选地,步骤(1)所述气相色谱法中采用的色谱仪型号为山东鲁南瑞虹SP-6890。
所述方法在步骤(2)之后还包括如下聚类分析的步骤:
米糠油掺棕榈油的聚类分析如下:将纯米糠油、纯棕榈油、待侧米糠油的脂肪酸C10:0、C14:0、C16:0、C16:1、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;从聚类群集表观察结果可知,9%以上掺伪量能予以鉴别;
米糠油掺菜籽油的聚类分析如下:将纯米糠油、纯菜籽油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C17:0、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1、C22:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;从聚类群集表观察结果可知,2%以上掺伪量能予以鉴别;
米糠油掺棉籽油的聚类分析如下:将纯米糠油、纯棉籽油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;从聚类群集表观察结果可知,5%以上掺伪量能予以鉴别;
米糠油掺大豆油的聚类分析如下:将纯米糠油、纯大豆油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C17:0、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1、C22:0的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;从聚类群集表观察结果可知,16%以上掺伪量能予以鉴别。
与现有技术相比,本发明建立了13个判别分析模型,判别分析模型为一元线性方程式,待侧样品检测省去了与标准植物油图谱比对及脂肪酸含量比对等步骤,直接将其脂肪酸比例代入即可鉴定植物油中掺伪油脂种类。本发明操作简单,计算方便,判别分析对市场上植物油进行检测准确率96%,可实现米糠油中掺棕榈油、菜籽油、棉籽油、大豆油、茶籽油、花生油的鉴定,检测准确率96%以上。米糠油掺棕榈油、菜籽油、棉籽油、大豆油的聚类分析能鉴别掺伪9%以上的棕榈油、掺伪2%以上的菜籽油、掺伪5%以上的棉籽油、掺伪16%以上的大豆油。
具体实施方式
实施例1
(1)色谱数据获取:待测植物油(实际为米糠油中掺入了24%的棕榈油)采用气相色谱法测定植物油中脂肪酸的含量,柱室220℃恒温。毛细管色谱柱。归一法计算各脂肪酸在植物油中的含量(质量百分比),结果见表1。
表1待测植物油(米糠油掺混棕榈油)的脂肪酸测定结果
(2)将待测植物油的脂肪酸含量代入以下13个计算模型中,计算Y1至Y13的数值结果:
Y1=949.821×C10:0+143.946×C14:0+89.515×C16:0+181.532×C16:1+359.968×C17:0+107.006×C18:0+101.592×C18:1+105.504×C18:2+93.738×C18:3+133.945×C20:0+140.364×C20:1+73.022×C22:0+55.167×C22:1-5031.548;
Y2=1438.311×C10:0+139.412×C14:0+91.792×C16:0+185.061×C16:1+361.166×C17:0+111.856×C18:0+100.457×C18:1+103.234×C18:2+94.770×C18:3+131.944×C20:0+138.912×C20:1+77.803×C22:0+55.222×C22:1-5049.374;
Y3=833.672×C10:0+134.870×C14:0+85.436×C16:0+172.626×C16:1+637.630×C17:0+98.978×C1 8:0+96.660×C18:1+98.821×C18:2+93.030×C18:3+144.994×C20:0+144.031×C20:1+66.448×C22:0+61.036×C22:1-4682.546;
Y4=896.353×C10:0+128.253×C14:0+84.320×C16:0+162.165×C16:1+384.505×C17:0+118.244×C18:0+101.018×C18:1+101.485×C18:2+89.035×C18:3+128.214×C20:0+136.708×C20:1+65.445×C22:0+50.248×C22:1-4852.422;
Y5=928.799×C10:0+152.520×C14:0+90.314×C16:0+189.679×C16:1+388.121×C17:0+114.050×C18:0+100.355×C18:1+106.986×C18:2+88.392×C18:3+122.661×C20:0+138.219×C20:1+71.585×C22:0+57.269×C22:1-5088.379;
Y6=910.200×C10:0+139.206×C14:0+89.538×C16:0+179.837×C16:1+377.844×C17:0+110.874×C18:0+101.812×C18:1+105.471×C18:2+91.924×C18:3+123.842×C20:0+145.055×C20:1+128.863×C22:0+52.648×C22:1-5159.902;
Y7=1040.664×C10:0+138.386×C14:0+89.206×C16:0+176.115×C16:1+446.255×C17:0+118.737×C18:0+101.533×C18:1+106.535×C18:2+104.723×C18:3+126.953×C20:0+137.938×C20:1+75.991×C22: 0+54.122×C22:1-5174.614;
Y8=1332.938×C10:0+141.742×C14:0+90.311×C16:0+180.668×C16:1+362.246×C17:0+111.429×C18:0+101.825×C18:1+105.543×C18:2+93.779×C18:3+134.566×C20:0+141.212×C20:1+72.544×C22:0+55.215×C22:1-5089.915;
Y9=900.173×C10:0+138.162×C14:0+87.246×C16:0+175.240×C16:1+487.459×C17:0+102.642×C18:0+99.064×C18:1+101.769×C18:2+94.465×C18:3+143.622×C20:0+147.800×C20:1+68.062×C22:0+56.071×C22:1-4816.328;
Y10=900.399×C10:0+136.828×C14:0+88.591×C16:0+177.154×C16:1+382.924×C17:0+113.400×C18:0+103.289×C18:1+104.908×C18:2+93.751×C18:3+131.177×C20:0+141.241×C20:1+73.050×C22:0+53.048×C22:1-5100.582;
Y11=934.574×C10:0+148.182×C14:0+90.524×C16:0+186.865×C16:1+374.092×C17:0+111.813×C18:0+101.489×C18:1+106.812×C18:2+91.637×C18:3+128.999×C20:0+140.408×C20:1+72.549×C22:0+56.431×C22:1-5107.566;
Y12=918.758×C10:0+140.704×C14:0+90.251×C16:0+181.331×C16:1+373.097×C17:0+112.340×C18:0+102.454×C18:1+106.129×C18:2+93.098×C18:3+135.285×C20:0+145.736×C20:1+99.281×C22:0+53.892×C22:1-5147.272;
Y13=949.965×C10:0+139.427×C14:0+90.171×C16:0+180.058×C16:1+454.214×C17:0+117.458×C18:0+102.039×C18:1+106.534×C18:2+100.227×C18:3+126.549×C20:0+140.273×C20:1+76.189×C22: 0+54.286×C22:1-5154.243;
其中,Y1表示米糠油,Y2表示棕榈油,Y3表示菜籽油,Y4表示茶籽油,Y5表示棉籽油,Y6表示花生油,Y7表示大豆油,Y8表示掺混棕榈油的米糠油,Y9表示掺混菜籽油的米糠油,Y10表示掺混茶籽油的米糠油,Y11表示掺混棉籽油的米糠油,Y12表示掺混花生油的米糠油,Y13表示掺混大豆油的米糠油;
若待测植物油的Y1至Y13中Y1的数值最大,则该植物油为米糠油;若Y2最大,则该植物油为棕榈油;若Y3最大,则该植物油为菜籽油;若Y4最大,则该植物油为茶籽油;若Y5最大,则该植物油为棉籽油;若Y6最大,则该植物油为花生油,若Y7最大,则该植物油为大豆油;若Y8最大,则该植物油为掺混棕榈油的米糠油;若Y9最大,则该植物油为掺混菜籽油的米糠油;若Y10最大,则该植物油为掺混茶籽油的米糠油;若Y11最大,则该植物油为掺混棉籽油的米糠油;若Y12最大,则该植物油为掺混花生油的米糠油;若Y13最大,则该植物油为掺混大豆油的米糠油。
表2显示最大的计算值为Y8(5231),因此该植物油判定为8掺混棕榈油的米糠油,与实际情况相吻合。
表2待测植物油(实际为米糠油中混入24%棕榈油)的判别分析值
函数 | Y1 | Y2 | Y3 | Y4 | Y5 | Y6 | Y7 |
计算值 | 5212 | 5170 | 5051 | 5124 | 5160 | 5079 | 5118 |
函数 | Y8 | Y9 | Y10 | Y11 | Y12 | Y13 | |
计算值 | 5231 | 5163 | 5180 | 5196 | 5181 | 5170 |
(3)米糠油掺棕榈油的聚类分析:将纯米糠油、8种掺混不同比例棕榈油的米糠油、待测米糠油(实际掺混24%的棕榈油)及纯棕榈油进行气相色谱分析,归一法测定共有脂肪酸的含量,SPSS进行聚类,结果见表3。表3显示群集为3、4时,掺伪量为18.1%以上的样品都纯米糠油(第1类)分开,为第2、3或4类。待测米糠油聚为2类,与掺混不同比例棕榈油的米糠油相同,可判断该米糠油为米糠油掺棕榈油。该方法在棕榈油掺伪18%及以上可以予以鉴别,掺伪7.34%以下不能进行辨别。进行7.34%-18%的验证试验,证明掺伪9%以上能予以鉴别。将判别分析与聚类分析相结合可提高鉴定的准确度。表3待测米糠油的聚类结果
本发明判别分析检测准确率96%,聚类分析能鉴别9%以上的棕榈油。
实施例2
(1)色谱数据获取:采用气相色谱法测定待测植物油(实际为米糠油中掺混11%的菜籽油)中脂肪酸的含量,柱室220℃恒温。毛细管色谱柱。外标法计算各脂肪酸在植物油中的含量(质量百分比),结果见表4。
表4待测植物油(米糠油掺混菜籽油)的脂肪酸测定结果
(2)将待测植物油的脂肪酸含量代入以下13个计算模型中,计算Y1至Y13的数值结果:
Y1=949.821×C10:0+143.946×C14:0+89.515×C16:0+181.532×C16:1+359.968×C17:0+107.006×C18:0+101.592×C18:1+105.504×C18:2+93.738×C18:3+133.945×C20:0+140.364×C20:1+73.022×C22:0+55.167×C22:1-5031.548;
Y2=1438.311×C10:0+139.412×C14:0+91.792×C16:0+185.061×C16:1+361.166×C17:0+111.856×C18:0+100.457×C18:1+103.234×C18:2+94.770×C18:3+131.944×C20:0+138.912×C20:1+77.803×C22:0+55.222×C22:1-5049.374;
Y3=833.672×C10:0+134.870×C14:0+85.436×C16:0+172.626×C16:1+637.630×C17:0+98.978×C1 8:0+96.660×C18:1+98.821×C18:2+93.030×C18:3+144.994×C20:0+144.031×C20:1+66.448×C22:0+61.036×C22:1-4682.546;
Y4=896.353×C10:0+128.253×C14:0+84.320×C16:0+162.165×C16:1+384.505×C17:0+118.244×C18:0+101.018×C18:1+101.485×C18:2+89.035×C18:3+128.214×C20:0+136.708×C20:1+65.445×C22:0+50.248×C22:1-4852.422;
Y5=928.799×C10:0+152.520×C14:0+90.314×C16:0+189.679×C16:1+388.121×C17:0+114.050×C18:0+100.355×C18:1+106.986×C18:2+88.392×C18:3+122.661×C20:0+138.219×C20:1+71.585×C22:0+57.269×C22:1-5088.379;
Y6=910.200×C10:0+139.206×C14:0+89.538×C16:0+179.837×C16:1+377.844×C17:0+110.874×C18:0+101.812×C18:1+105.471×C18:2+91.924×C18:3+123.842×C20:0+145.055×C20:1+128.863×C22:0+52.648×C22:1-5159.902;
Y7=1040.664×C10:0+138.386×C14:0+89.206×C16:0+176.115×C16:1+446.255×C17:0+118.737×C18:0+101.533×C18:1+106.535×C18:2+104.723×C18:3+126.953×C20:0+137.938×C20:1+75.991×C22: 0+54.122×C22:1-5174.614;
Y8=1332.938×C10:0+141.742×C14:0+90.311×C16:0+180.668×C16:1+362.246×C17:0+111.429×C18:0+101.825×C18:1+105.543×C18:2+93.779×C18:3+134.566×C20:0+141.212×C20:1+72.544×C22:0+55.215×C22:1-5089.915;
Y9=900.173×C10:0+138.162×C14:0+87.246×C16:0+175.240×C16:1+487.459×C17:0+102.642×C18:0+99.064×C18:1+101.769×C18:2+94.465×C18:3+143.622×C20:0+147.800×C20:1+68.062×C22:0+56.071×C22:1-4816.328;
Y10=900.399×C10:0+136.828×C14:0+88.591×C16:0+177.154×C16:1+382.924×C17:0+113.400×C18:0+103.289×C18:1+104.908×C18:2+93.751×C18:3+131.177×C20:0+141.241×C20:1+73.050×C22:0+53.048×C22:1-5100.582;
Y11=934.574×C10:0+148.182×C14:0+90.524×C16:0+186.865×C16:1+374.092×C17:0+111.813×C18:0+101.489×C18:1+106.812×C18:2+91.637×C18:3+128.999×C20:0+140.408×C20:1+72.549×C22:0+56.431×C22:1-5107.566;
Y12=918.758×C10:0+140.704×C14:0+90.251×C16:0+181.331×C16:1+373.097×C17:0+112.340×C18:0+102.454×C18:1+106.129×C18:2+93.098×C18:3+135.285×C20:0+145.736×C20:1+99.281×C22:0+53.892×C22:1-5147.272;
Y13=949.965×C10:0+139.427×C14:0+90.171×C16:0+180.058×C16:1+454.214×C17:0+117.458×C18:0+102.039×C18:1+106.534×C18:2+100.227×C18:3+126.549×C20:0+140.273×C20:1+76.189×C22: 0+54.286×C22:1-5154.243;
其中,Y1表示米糠油,Y2表示棕榈油,Y3表示菜籽油,Y4表示茶籽油,Y5表示棉籽油,Y6表示花生油,Y7表示大豆油,Y8表示掺混棕榈油的米糠油,Y9表示掺混菜籽油的米糠油,Y10表示掺混茶籽油的米糠油,Y11表示掺混棉籽油的米糠油,Y12表示掺混花生油的米糠油,Y13表示掺混大豆油的米糠油;
若待测植物油的Y1至Y13中Y1的数值最大,则该植物油为米糠油;若Y2最大,则该植物油为棕榈油;若Y3最大,则该植物油为菜籽油;若Y4最大,则该植物油为茶籽油;若Y5最大,则该植物油为棉籽油;若Y6最大,则该植物油为花生油,若Y7最大,则该植物油为大豆油;若Y8最大,则该植物油为掺混棕榈油的米糠油;若Y9最大,则该植物油为掺混菜籽油的米糠油;若Y10最大,则该植物油为掺混茶籽油的米糠油;若Y11最大,则该植物油为掺混棉籽油的米糠油;若Y12最大,则该植物油为掺混花生油的米糠油;若Y13最大,则该植物油为掺混大豆油的米糠油。
表5显示最大的计算值为Y9(4543),因此该植物油判定为9掺混菜籽油的米糠油,与实际情况相吻合。
表5待测植物油(实际为米糠油中混入11%菜籽油)的判别分析值
函数 | Y1 | Y2 | Y3 | Y4 | Y5 | Y6 | Y7 |
计算值 | 4530 | 4436 | 4463 | 4465 | 4454 | 4398 | 4424 |
函数 | Y8 | Y9 | Y10 | Y11 | Y12 | Y13 | |
计算值 | 4511 | 4543 | 4499 | 4498 | 4499 | 4475 |
(3)米糠油掺菜籽油的聚类分析:将纯米糠油、8种掺混不同比例菜籽油的米糠油、待测米糠油(实际掺混11%的菜籽油)及纯菜籽油进行气相色谱分析,归一法测定共有脂肪酸的含量,SPSS进行聚类,结果见表6。表6显示群集为3、4时,掺伪量为11.4%以上的样品都纯米糠油(第1类)分开,为第2、3或4类。待测米糠油聚为2、3类,与掺混不同比例菜籽油的米糠油相同,可判断该米糠油为米糠油掺菜籽油。该方法在菜籽油掺伪11.4%及以上可以予以鉴别,对11.4%以下的进行验证试验,表明2%以上即能区别于纯米糠油。该方法明显优于化学分析法。
将判别分析与聚类分析相结合可提高鉴定的准确度。
表6待测米糠油(米糠油掺混11%菜籽油)的聚类结果
本发明判别分析检测准确率96.5%,聚类分析能鉴别2%以上的菜籽油。
Claims (3)
1.一种利用化学计量法定性检测植物油中掺伪油脂的方法,其特征在于,所述方法包括如下步骤:
(1)采用气相色谱法测定待测植物油中各脂肪酸的含量;
(2)将待测植物油的脂肪酸含量代入以下13个计算模型中,计算Y1至Y13的数值结果:
Y1=949.821×C10:0+143.946×C14:0+89.515×C16:0+181.532×C16:1+359.968×C17:0+107.006×C18:0+101.592×C18:1+105.504×C18:2+93.738×C18:3+133.945×C20:0+140.364×C20:1+73.022×C22:0+55.167×C22:1-5031.548;
Y2=1438.311×C10:0+139.412×C14:0+91.792×C16:0+185.061×C16:1+361.166×C17:0+111.856×C18:0+100.457×C18:1+103.234×C18:2+94.770×C18:3+131.944×C20:0+138.912×C20:1+77.803×C22:0+55.222×C22:1-5049.374;
Y3=833.672×C10:0+134.870×C14:0+85.436×C16:0+172.626×C16:1+637.630×C17:0+98.978×C1 8:0+96.660×C18:1+98.821×C18:2+93.030×C18:3+144.994×C20:0+144.031×C20:1+66.448×C22:0+61.036×C22:1-4682.546;
Y4=896.353×C10:0+128.253×C14:0+84.320×C16:0+162.165×C16:1+384.505×C17:0+118.244×C18:0+101.018×C18:1+101.485×C18:2+89.035×C18:3+128.214×C20:0+136.708×C20:1+65.445×C22:0+50.248×C22:1-4852.422;
Y5=928.799×C10:0+152.520×C14:0+90.314×C16:0+189.679×C16:1+388.121×C17:0+114.050×C18:0+100.355×C18:1+106.986×C18:2+88.392×C18:3+122.661×C20:0+138.219×C20:1+71.585×C22:0+57.269×C22:1-5088.379;
Y6=910.200×C10:0+139.206×C14:0+89.538×C16:0+179.837×C16:1+377.844×C17:0+110.874×C18:0+101.812×C18:1+105.471×C18:2+91.924×C18:3+123.842×C20:0+145.055×C20:1+128.863×C22:0+52.648×C22:1-5159.902;
Y7=1040.664×C10:0+138.386×C14:0+89.206×C16:0+176.115×C16:1+446.255×C17:0+118.737×C18:0+101.533×C18:1+106.535×C18:2+104.723×C18:3+126.953×C20:0+137.938×C20:1+75.991×C22: 0+54.122×C22:1-5174.614;
Y8=1332.938×C10:0+141.742×C14:0+90.311×C16:0+180.668×C16:1+362.246×C17:0+111.429×C18:0+101.825×C18:1+105.543×C18:2+93.779×C18:3+134.566×C20:0+141.212×C20:1+72.544×C22:0+55.215×C22:1-5089.915;
Y9=900.173×C10:0+138.162×C14:0+87.246×C16:0+175.240×C16:1+487.459×C17:0+102.642×C18:0+99.064×C18:1+101.769×C18:2+94.465×C18:3+143.622×C20:0+147.800×C20:1+68.062×C22:0+56.071×C22:1-4816.328;
Y10=900.399×C10:0+136.828×C14:0+88.591×C16:0+177.154×C16:1+382.924×C17:0+113.400×C18:0+103.289×C18:1+104.908×C18:2+93.751×C18:3+131.177×C20:0+141.241×C20:1+73.050×C22:0+53.048×C22:1-5100.582;
Y11=934.574×C10:0+148.182×C14:0+90.524×C16:0+186.865×C16:1+374.092×C17:0+111.813×C18:0+101.489×C18:1+106.812×C18:2+91.637×C18:3+128.999×C20:0+140.408×C20:1+72.549×C22:0+56.431×C22:1-5107.566;
Y12=918.758×C10:0+140.704×C14:0+90.251×C16:0+181.331×C16:1+373.097×C17:0+112.340×C18:0+102.454×C18:1+106.129×C18:2+93.098×C18:3+135.285×C20:0+145.736×C20:1+99.281×C22:0+53.892×C22:1-5147.272;
Y13=949.965×C10:0+139.427×C14:0+90.171×C16:0+180.058×C16:1+454.214×C17:0+117.458×C18:0+102.039×C18:1+106.534×C18:2+100.227×C18:3+126.549×C20:0+140.273×C20:1+76.189×C22: 0+54.286×C22:1-5154.243;
其中,Y1表示米糠油,Y2表示棕榈油,Y3表示菜籽油,Y4表示茶籽油,Y5表示棉籽油,Y6表示花生油,Y7表示大豆油,Y8表示掺混棕榈油的米糠油,Y9表示掺混菜籽油的米糠油,Y10表示掺混茶籽油的米糠油,Y11表示掺混棉籽油的米糠油,Y12表示掺混花生油的米糠油,Y13表示掺混大豆油的米糠油;
若待测植物油的Y1至Y13中Y1的数值最大,则该植物油为米糠油;若Y2最大,则该植物油为棕榈油;若Y3最大,则该植物油为菜籽油;若Y4最大,则该植物油为茶籽油;若Y5最大,则该植物油为棉籽油;若Y6最大,则该植物油为花生油,若Y7最大,则该植物油为大豆油;若Y8最大,则该植物油为掺混棕榈油的米糠油;若Y9最大,则该植物油为掺混菜籽油的米糠油;若Y10最大,则该植物油为掺混茶籽油的米糠油;若Y11最大,则该植物油为掺混棉籽油的米糠油;若Y12最大,则该植物油为掺混花生油的米糠油;若Y13最大,则该植物油为掺混大豆油的米糠油。
2.如权利要求1所述的方法,其特征在于,步骤(1)所述气相色谱法中采用的色谱仪型号为山东鲁南瑞虹SP-6890。
3.如权利要求1或2所述的方法,其特征在于,所述方法在步骤(2)之后还包括如下聚类分析的步骤:
米糠油掺棕榈油的聚类分析如下:将纯米糠油、纯棕榈油、待侧米糠油的脂肪酸C10:0、C14:0、C16:0、C16:1、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;
米糠油掺菜籽油的聚类分析如下:将纯米糠油、纯菜籽油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C17:0、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1、C22:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;
米糠油掺棉籽油的聚类分析如下:将纯米糠油、纯棉籽油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4;
米糠油掺大豆油的聚类分析如下:将纯米糠油、纯大豆油、待侧米糠油的脂肪酸C14:0、C16:0、C16:1、C17:0、C18:0、C18:1、C18:2、C18:3、C20:0、C20:1、C22:0的含量作为变量,用SPSS软件进行聚类,选择聚类群集数为2~4。
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