不同研磨条件对玉米样品粉碎制备效果的影响
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摘要
目的研究不同研磨条件粉碎玉米样品的效果,科学制备样品。方法使用平行研磨仪对玉米样品进行粉碎,分别考察不同重量、不同研磨时间、不同循环次数下粉碎后的玉米通过20目、40目、60目标准筛的过筛率,幵采用QuEChERS-超高效液相色谱-串联质谱法测定不同粉碎条件的样品添加回收结果,来辅助评价研磨效果。结果 50g玉米样品研磨60s循环1次后过20目筛率可达71.8%,未过筛直接添加26种农药回收率为74.4%～114.0%[除甲胺磷外,相对标准偏差(relative standard deviation,RSD)为1.8%～8.5%];100 g玉米研磨30 s循环2次后过20目筛率为58.0%,未过筛直接添加26种农药回收率为77.7%～118.1%(除甲胺磷外, RSD为1.5%～10.3%)。结论实验使用的平行研磨仪适用于多个玉米样品同时粉碎制备,相比传统研磨仪只能逐个粉碎样品的处理效率得到显著提高,一次性研磨50～100 g玉米60 s后即可满足科学制备检测样品的需要。
Objective To investigate the effect of different grinding conditions on the smash effect of corn sample, in order to prepare samples scientifically. Methods The corn sample was pulverized by a parallel grinder,the sieving rate of the pulverized corn through 20-mesh, 40-mesh, and 60-mesh standard sieves under different weights, different grinding times, and different cycle times was examined, and the standard recovery rates under different pulverization conditions were determined to assist in the evaluation of the grinding effect by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Results The 50 g corn sample was ground for 60 s once and then passed through a 20-mesh sieve for 71.8%. The recovery rate of 26 pesticides added directly without screening was 74.4%-114.0% [except for methamidophos, the relative standard deviation(RSD) was 1.8%-8.5%]; The 100 g corn sample was ground for 30 s for 2 times and then passed through a 20-mesh sieve for 58.0%. The recovery rate of 26 pesticides without screening was 77.7%-118.1%(except for methamidophos,RSD was 1.5%-10.3%). Conclusion The parallel grinder used in the test is suitable for simultaneous pulverization of multiple corn samples, and obviously improve the efficiency compared to traditional methods which can only grind samples one by one. Grinding 50-100 g corn for 60 s at a time can meet the needs of scientific preparation of test samples.
Objective To investigate the effect of different grinding conditions on the smash effect of corn sample, in order to prepare samples scientifically. Methods The corn sample was pulverized by a parallel grinder,the sieving rate of the pulverized corn through 20-mesh, 40-mesh, and 60-mesh standard sieves under different weights, different grinding times, and different cycle times was examined, and the standard recovery rates under different pulverization conditions were determined to assist in the evaluation of the grinding effect by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry. Results The 50 g corn sample was ground for 60 s once and then passed through a 20-mesh sieve for 71.8%. The recovery rate of 26 pesticides added directly without screening was 74.4%-114.0% [except for methamidophos, the relative standard deviation(RSD) was 1.8%-8.5%]; The 100 g corn sample was ground for 30 s for 2 times and then passed through a 20-mesh sieve for 58.0%. The recovery rate of 26 pesticides without screening was 77.7%-118.1%(except for methamidophos,RSD was 1.5%-10.3%). Conclusion The parallel grinder used in the test is suitable for simultaneous pulverization of multiple corn samples, and obviously improve the efficiency compared to traditional methods which can only grind samples one by one. Grinding 50-100 g corn for 60 s at a time can meet the needs of scientific preparation of test samples.
引文
[1]金芳.浅谈食品检验前样品的制备与保存[J].科技风,2009,(21):183.Jin F.Preparation and preservation of samples before food inspection[J].Technol Trend,2009,(21):183.
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[3]王济世,贺泽英,徐亚平,等.自动Qu EChERS方法结合液相色谱串联质谱对玉米中133种农药的多残留分析[J].农业环境科学学报,2018,(3703):605-612.Wang JS,He ZY,Xu YP,et al.Multiresidue analysis of 133 pesticides in corn using automatic QuEChERS with LC-MS/MS[J].J Agro-Environ Sci,2018,(3703):605-612.
[4]杨晓慧.浅议食品卫生检验样品的采集、制备和保存[J].中国农业信息,2015,(9):131.Yang XH.Discussion on the collection,preparation and preservation of food hygiene inspection samples[J].China Agric Inform,2015,(9):131.
[5]易善平,金俊节,乔青青,等.实验室食品检测样品的管理和控制[J].食品安全导刊,2017,(12):154-156.Yi SP,Jin JJ,Qiao QQ,et al.Management and control of laboratory food test samples[J].China Food Saf Mag,2017,(12):154-156.
[6]滕金兰.检验室食品样品制备管理[J].广西轻工业,2010,(7):19-20.Teng JL.Food sample preparation management in inspection room[J].Guangxi J Light Ind,2010,(7):19-20.
[7]GB/T 5009.1-2003食品卫生检验方法理化部分[S].GB/T 5009.1-2003 Methods of food hygienic analysis-Physical and chemical section-General principles[S].
[8]王竹天,兰真,鲁杰,等.GBT5009-2003《食品卫生检验方法》理化部分简介[J].中国食品卫生杂志,2005,(3):193-211.Wang ZT,Lan Z,Lu J,et al.Introduction of GB/T 5009-2003 Methods of food hygienic analysis-physical and chemical section[J].Chin J Food Hyg,2005,(3):193-211.
[9]GB/T 20770-2008粮谷中486种农药及相兲化学品残留量的测定液相色谱串联质谱法[S].GB/T 20770-2008 Determination of 486 pesticides and related chemicals residues in grains-LC-MS-MS method[S].
[10]GB 23200.9-2016食品安全国家标准粮谷中475种农药及相兲化学品残留量的测定气相色谱-质谱法[S].GB 23200.9-2016 National food safety standard-Method for determination of 475 pesticides and related chemicals residues in grains-GC-MS method[S].
[11]GB 23200.33-2016食品安全国家标准食品中解草嗪、莎稗磷、二丙烯草胺等110种农药残留量的测定气相色谱-质谱法[S].GB 23200.33-2016 National food safety standards-Determination of benoxacor,anilofos,allidochlor 110 pesticides residues in foods-Gas chromatography-mass spectrometry[S].
[12]GB 23200.37-2016食品安全国家标准食品中烯啶虫胺、呋虫胺等20种农药残留量的测定液相色谱-质谱质谱法[S].GB 23200.37-2016 National food safety standards-Determination of residue of 20 pesticides including nitenpyram,dinotefuranetc in foods-Liquid chromatography-tandem mass spectrometry[S].
[13]GB 23200.113-2018食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱-质谱联用法[S].GB 23200.113-2018 National food safety standard-Determination of 208pesticides and metabolites residues in foods of plant origin-Gas chromatography-tandem mass spectrometry method[S].
[14]GB/T 36858-2018饲料中黄曲霉毒素B1的测定高效液相色谱法[S].GB/T 36858-2018 Determination of aflatoxin B1 in feeds-High performance liquid chromatography[S].
[15]DB 34/T 2406-2015大米中17种农药残留量的测定液相色谱-串联质谱法[S].DB 34/T 2406-2015 Determination of 17 pesticides residues in rice-Lquid chromatography tandem mass spectrometry[S].
[16]González-Curbelo Má,Lehotay SJ,Hernández-Borges J,et al.Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast,low-pressure gas chromatography and liquid chromatography tandem mass spectrometry[J].J Chromatogr A,2014,(1358):75-84.
[17]He Z,Wang L,Peng Y,et al.Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chem,2015,(169):372-380.
[18]Dzuman Z,Zachariasova M,Veprikova Z,et al.Multi-analyte high performance liquid chromatography coupled to high resolution tandem mass spectrometry method for control of pesticide residues,mycotoxins,and pyrrolizidine alkaloids[J].Anal Chim Acta,2015,(863):29-40.
[19]Lee YJ,Rahman MM,El-Aty AMA,et al.Detection of three herbicide,and one metabolite,residues in brown rice and rice straw using various versions of the QuEChERS method and liquid chromatography-tandem mass spectrometry[J].Food Chem,2016,(210):442-450.
[20]王连珠,黄小燕,王登飞,等.QuEChERS-液相色谱-串联质谱法测定甜玉米及毛豆中32种磺酰脲类除草剂残留[J].色谱,2015,33(5):501-507.Wang LZ,Huang XY,Wang DF,et al.Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry[J].Chin JChromatogr,2015,33(5):501-507.
[21]王婧.QuEChERS前处理方法在农药残留检测中的应用[J].山西农业科学,2017,(4512):2051-2055.Wang J.Study on the application of QuEChERS pretreatment method in the detection of pesticide residues[J].J Shanxi Agric Sci,2017,(4512):2051-2055.
[22]王纯强,钱永忠,章程辉,等.QuEChERS-超高效液相色谱-QDa质谱法快速测定白菜与油菜中15种氨基甲酸酯类农药及代谢物残留[J].农药学学报,2018,20(4):459-467.Wang CQ,Qian YZ,Zhang CH,et al.Residue determination of 15carbamates and their metabolites in Chinese cabages and pakchoi by QuEChERS-ultra high performance liquid chromatography-QDa mass spectrometry[J].Chin J Pestic Sci,2018,20(4):459-467.
[23]畅晓晖.刀式混合研磨仪GM200在样品制备中的应用研究[J].食品安全质量检测学报,2015,(611):4358-4365.Chang XH.Application of retsch grindomix GM200 on food sample preparation[J].J Food Saf Qual,2015,(611):4358-4365.
[24]董亮,张赞蓉.粉碎技术在样品前处理中的应用-利用RETSCH研磨粉碎仪器获得有代表性的样品[J].食品安全导刊,2011,(11):34-35.Dong L,Zhang ZR.Application of crushing technology in sample pretreatment-using RETSCH grinding crushing instrument to obtain representative samples[J].China Food Saf Mag,2011,(11):34-35.
[25]回瑞华,侯冬岩,刁全平,等.样品粉碎粒度不同对挥发油提取作用的影响研究[J].鞍山师范学院学报,2015,(1704):29-32.Hui RH,Hou DY,Diao QP,et al.Sample granularity of the influence of different effect on volatile oil extraction research[J].J Anshan Normal Univ,2015,(1704):29-32.
[26]Mahugija JAM,Kayombo A,Peter R.Pesticide residues in raw and processed maize grains and flour from selected areas in Dar es Salaam and Ruvuma,Tanzania[J].Chemosphere,2017,(185):137-144.
[2]杨益军.中国三大粮食作物农药使用情况深度分析及问题探讨[J].农药市场信息,2015,(26):31-35.Yang YJ.In-depth analysis and discussion on pesticide use of China's three major grain crops[J].Pestic Market News,2015,(26):31-35.
[3]王济世,贺泽英,徐亚平,等.自动Qu EChERS方法结合液相色谱串联质谱对玉米中133种农药的多残留分析[J].农业环境科学学报,2018,(3703):605-612.Wang JS,He ZY,Xu YP,et al.Multiresidue analysis of 133 pesticides in corn using automatic QuEChERS with LC-MS/MS[J].J Agro-Environ Sci,2018,(3703):605-612.
[4]杨晓慧.浅议食品卫生检验样品的采集、制备和保存[J].中国农业信息,2015,(9):131.Yang XH.Discussion on the collection,preparation and preservation of food hygiene inspection samples[J].China Agric Inform,2015,(9):131.
[5]易善平,金俊节,乔青青,等.实验室食品检测样品的管理和控制[J].食品安全导刊,2017,(12):154-156.Yi SP,Jin JJ,Qiao QQ,et al.Management and control of laboratory food test samples[J].China Food Saf Mag,2017,(12):154-156.
[6]滕金兰.检验室食品样品制备管理[J].广西轻工业,2010,(7):19-20.Teng JL.Food sample preparation management in inspection room[J].Guangxi J Light Ind,2010,(7):19-20.
[7]GB/T 5009.1-2003食品卫生检验方法理化部分[S].GB/T 5009.1-2003 Methods of food hygienic analysis-Physical and chemical section-General principles[S].
[8]王竹天,兰真,鲁杰,等.GBT5009-2003《食品卫生检验方法》理化部分简介[J].中国食品卫生杂志,2005,(3):193-211.Wang ZT,Lan Z,Lu J,et al.Introduction of GB/T 5009-2003 Methods of food hygienic analysis-physical and chemical section[J].Chin J Food Hyg,2005,(3):193-211.
[9]GB/T 20770-2008粮谷中486种农药及相兲化学品残留量的测定液相色谱串联质谱法[S].GB/T 20770-2008 Determination of 486 pesticides and related chemicals residues in grains-LC-MS-MS method[S].
[10]GB 23200.9-2016食品安全国家标准粮谷中475种农药及相兲化学品残留量的测定气相色谱-质谱法[S].GB 23200.9-2016 National food safety standard-Method for determination of 475 pesticides and related chemicals residues in grains-GC-MS method[S].
[11]GB 23200.33-2016食品安全国家标准食品中解草嗪、莎稗磷、二丙烯草胺等110种农药残留量的测定气相色谱-质谱法[S].GB 23200.33-2016 National food safety standards-Determination of benoxacor,anilofos,allidochlor 110 pesticides residues in foods-Gas chromatography-mass spectrometry[S].
[12]GB 23200.37-2016食品安全国家标准食品中烯啶虫胺、呋虫胺等20种农药残留量的测定液相色谱-质谱质谱法[S].GB 23200.37-2016 National food safety standards-Determination of residue of 20 pesticides including nitenpyram,dinotefuranetc in foods-Liquid chromatography-tandem mass spectrometry[S].
[13]GB 23200.113-2018食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱-质谱联用法[S].GB 23200.113-2018 National food safety standard-Determination of 208pesticides and metabolites residues in foods of plant origin-Gas chromatography-tandem mass spectrometry method[S].
[14]GB/T 36858-2018饲料中黄曲霉毒素B1的测定高效液相色谱法[S].GB/T 36858-2018 Determination of aflatoxin B1 in feeds-High performance liquid chromatography[S].
[15]DB 34/T 2406-2015大米中17种农药残留量的测定液相色谱-串联质谱法[S].DB 34/T 2406-2015 Determination of 17 pesticides residues in rice-Lquid chromatography tandem mass spectrometry[S].
[16]González-Curbelo Má,Lehotay SJ,Hernández-Borges J,et al.Use of ammonium formate in QuEChERS for high-throughput analysis of pesticides in food by fast,low-pressure gas chromatography and liquid chromatography tandem mass spectrometry[J].J Chromatogr A,2014,(1358):75-84.
[17]He Z,Wang L,Peng Y,et al.Multiresidue analysis of over 200 pesticides in cereals using a QuEChERS and gas chromatography-tandem mass spectrometry-based method[J].Food Chem,2015,(169):372-380.
[18]Dzuman Z,Zachariasova M,Veprikova Z,et al.Multi-analyte high performance liquid chromatography coupled to high resolution tandem mass spectrometry method for control of pesticide residues,mycotoxins,and pyrrolizidine alkaloids[J].Anal Chim Acta,2015,(863):29-40.
[19]Lee YJ,Rahman MM,El-Aty AMA,et al.Detection of three herbicide,and one metabolite,residues in brown rice and rice straw using various versions of the QuEChERS method and liquid chromatography-tandem mass spectrometry[J].Food Chem,2016,(210):442-450.
[20]王连珠,黄小燕,王登飞,等.QuEChERS-液相色谱-串联质谱法测定甜玉米及毛豆中32种磺酰脲类除草剂残留[J].色谱,2015,33(5):501-507.Wang LZ,Huang XY,Wang DF,et al.Determination of 32 sulfonylurea herbicide residues in sweet corns and green soybeans by QuEChERS-liquid chromatography-tandem mass spectrometry[J].Chin JChromatogr,2015,33(5):501-507.
[21]王婧.QuEChERS前处理方法在农药残留检测中的应用[J].山西农业科学,2017,(4512):2051-2055.Wang J.Study on the application of QuEChERS pretreatment method in the detection of pesticide residues[J].J Shanxi Agric Sci,2017,(4512):2051-2055.
[22]王纯强,钱永忠,章程辉,等.QuEChERS-超高效液相色谱-QDa质谱法快速测定白菜与油菜中15种氨基甲酸酯类农药及代谢物残留[J].农药学学报,2018,20(4):459-467.Wang CQ,Qian YZ,Zhang CH,et al.Residue determination of 15carbamates and their metabolites in Chinese cabages and pakchoi by QuEChERS-ultra high performance liquid chromatography-QDa mass spectrometry[J].Chin J Pestic Sci,2018,20(4):459-467.
[23]畅晓晖.刀式混合研磨仪GM200在样品制备中的应用研究[J].食品安全质量检测学报,2015,(611):4358-4365.Chang XH.Application of retsch grindomix GM200 on food sample preparation[J].J Food Saf Qual,2015,(611):4358-4365.
[24]董亮,张赞蓉.粉碎技术在样品前处理中的应用-利用RETSCH研磨粉碎仪器获得有代表性的样品[J].食品安全导刊,2011,(11):34-35.Dong L,Zhang ZR.Application of crushing technology in sample pretreatment-using RETSCH grinding crushing instrument to obtain representative samples[J].China Food Saf Mag,2011,(11):34-35.
[25]回瑞华,侯冬岩,刁全平,等.样品粉碎粒度不同对挥发油提取作用的影响研究[J].鞍山师范学院学报,2015,(1704):29-32.Hui RH,Hou DY,Diao QP,et al.Sample granularity of the influence of different effect on volatile oil extraction research[J].J Anshan Normal Univ,2015,(1704):29-32.
[26]Mahugija JAM,Kayombo A,Peter R.Pesticide residues in raw and processed maize grains and flour from selected areas in Dar es Salaam and Ruvuma,Tanzania[J].Chemosphere,2017,(185):137-144.
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