糧油檢驗(yàn)馬鈴薯及其制品中龍葵素的測(cè)定高效液相色譜-串聯(lián)質(zhì)譜法編制說(shuō)明

1《糧油檢驗(yàn)馬鈴薯及其制品中龍葵素的測(cè)定高效液相色譜-串聯(lián)質(zhì)譜法》編制說(shuō)明牽頭負(fù)責(zé)開(kāi)展《糧油檢驗(yàn)馬鈴薯及其制品中龍葵素的測(cè)定高效液相色譜-串聯(lián)2015年開(kāi)始我國(guó)啟動(dòng)馬鈴薯主糧化戰(zhàn)略，馬鈴薯成為小麥我國(guó)食品安全檢驗(yàn)標(biāo)準(zhǔn)和糧油質(zhì)量檢驗(yàn)標(biāo)準(zhǔn)中2光度法、薄層色譜法、高效液相色譜法、液相色譜-質(zhì)質(zhì)干擾的影響，還可以完成“-茄堿和“-卡茄堿的同時(shí)檢測(cè)，可為低含量龍葵素32．標(biāo)準(zhǔn)編制原則和確定標(biāo)準(zhǔn)主要內(nèi)容（如技術(shù)指標(biāo)、2.2確定標(biāo)準(zhǔn)的主要內(nèi)容本標(biāo)準(zhǔn)規(guī)定了高效液相色譜-串聯(lián)質(zhì)譜法測(cè)定馬鈴薯及其制品中龍葵素（“-42.3確定標(biāo)準(zhǔn)主要內(nèi)容的論據(jù)應(yīng)離子對(duì)的錐孔電壓和碰撞能量等質(zhì)譜參數(shù)，并選擇相對(duì)豐度值更高的子離子5利于離子在流動(dòng)相中的形成，并且易揮發(fā)。實(shí)驗(yàn)比較了0.1%甲酸水/乙腈、10作為流動(dòng)相，龍葵素的離子化效果均較好于0.1%甲酸6現(xiàn)，試樣通過(guò)提取液提取后，在甲醇溶液中沉降速度準(zhǔn)曲線。線性回歸方程為：α-茄堿Y=308.41X-166.30；R2=0.9925。α-卡茄堿 y=308.410452*x-166.300505R^2=0.99251901Type:Linear,Origin:Include,Weight:1/x y=308.410452*x-166.300505R^2=0.99251901Type:Linear,Origin:Include,Weight:1/xx10x10 2.25 0 -0.25-50510Concentration(ng/ml)7x10 y=183.489954*x-142.302851R^2=0.99349266Type:Linear,Origin:Include,Weight:1/x 0054045Concentration(ng/ml)實(shí)際測(cè)得值（ng/mL）品中的理論含量比827404—2008《實(shí)驗(yàn)室質(zhì)量控制規(guī)范食品理化檢測(cè)》的技術(shù)要求，表明方法具有編號(hào)稱(chēng)樣量定容體對(duì)照品濃度(μg/mL）加標(biāo)量數(shù)折算到樣品中的理論含量（mg/kg）實(shí)際測(cè)得折算到樣品中的實(shí)際含量（mg/kg）回收率(%)回收率平均值（%)RSD樣品/25.00///0.916////25.00///1.064///回收率（低）L-11.125425.008.05810.76019.561106.4105.84.5L-21.114225.008.13910.31359.256101.6L-31.015425.008.93110.939510.774109.5L-41.120425.008.09410.11499.02899.3L-51.230525.007.37011.37669.246112.0L-61.001525.009.05510.619210.603106.2回收率（中）M-10.958725.002523.64820.347421.22485.688.25.6M-21.002525.002522.61422.351022.29594.2M-30.994525.002522.79619.557719.66681.9M-41.002425.002522.61720.736120.68687.1M-51.021525.002522.19422.354421.88494.1M-60.945125.002523.98820.515421.70786.4回收率（高）H-11.015425.007566.98165.941864.94295.593.32.0H-21.000125.007568.00664.247664.24193.0H-30.957425.007571.03962.084764.84789.9H-40.956325.007571.12164.930967.89894.1H-50.999225.007568.06764.472164.52493.3H-61.001925.007567.88464.911764.78994.0編號(hào)稱(chēng)樣量定容體對(duì)照品濃度(μg/mL）加標(biāo)量數(shù)折算到樣品中的理論含量（mg/kg）實(shí)際測(cè)得折算到樣品中的實(shí)際含量（mg/kg）回收率(%)回收率平均值（%)RSD樣品/25.00///1.380////25.00///1.380///回收率（低）L-11.125425.009.45413.991012.432116.9119.63.6L-21.114225.009.54913.633012.236117.8L-31.015425.0010.47914.216614.001124.2L-41.120425.009.49713.988712.485121.0L-51.230525.008.64714.827812.050127.9L-61.001525.0010.62413.617113.597118.7回收率（中）M-10.958725.002527.74628.029529.237101.8109.64.3M-21.002525.002526.53430.848830.772112.2M-30.994525.002526.74731.457431.631114.6M-41.002425.002526.53629.208829.139106.1M-51.021525.002526.04030.461929.821110.7M-60.945125.002528.14530.815632.606112.3回收率（高）H-11.015425.007578.59078.702677.50997.493.72.3H-21.000125.007579.79275.611175.60493.5H-30.957425.007583.35174.343277.65192.0H-40.956325.007583.44774.549977.95792.2H-50.999225.007579.86474.540174.60092.2H-61.001925.007579.64976.994676.84995.23.主要試驗(yàn)（或驗(yàn)證）情況的分析、綜述報(bào)告，技術(shù)經(jīng)濟(jì)論證，預(yù)期的經(jīng)本標(biāo)準(zhǔn)建立了采用酸化乙腈提取，高效液相色譜4．與國(guó)際、國(guó)外對(duì)比情況（采用國(guó)際標(biāo)準(zhǔn)和國(guó)外先進(jìn)標(biāo)準(zhǔn)的程度，以及與馬鈴薯中龍葵素常用的檢測(cè)方法