CN112444591B - 一种测定植物性食品中唑嘧菌胺残留量的液相色谱串联质谱法 - Google Patents
一种测定植物性食品中唑嘧菌胺残留量的液相色谱串联质谱法 Download PDFInfo
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Abstract
本发明属于食品安全技术领域，涉及一种测定植物性食品中唑嘧菌胺残留量的液相色谱串联质谱法。称取均匀样品，以甲醇均质提取，无水硫酸镁和PSA净化，高速冷冻离心后，上清液旋蒸至近干，80％乙腈溶解残渣，过Oasis PRiME HLB柱净化，经0.22μm滤膜过滤，经液相色谱串联质谱检测，外标法定量。本发明所述检测方法前处理步骤简单新颖，除杂效果好，方法的灵敏度、回收率高，测定结果的精密度好，可以有效的检测植物性食品中唑嘧菌胺残留量。
Description
技术领域
本发明属于食品安全技术领域，具体涉及一种液相色谱串联质谱测定植物性食品中唑嘧菌胺残留量的方法。
技术背景
唑嘧菌胺是一个三唑嘧啶类杀菌剂，属于线粒体呼吸抑制剂，是一种高选择性的杀菌剂，对霜霉和疫霉类卵菌纲真菌有控制作用，具有极强的残留活性和耐雨性，能在叶片中重新分布，保护作物健康成长，充分发挥生长潜力。2010年初，唑嘧菌胺在罗马尼亚首先获得登记，主要用于防治葡萄上的晚疫病及霜霉病；2010年7月，在英国获准登记；同年，在荷兰取得登记；2011年，唑嘧菌胺产品Initium上市；2012年，在澳大利亚、加拿大、意大利和美国登记，用于果树、蔬菜、啤酒花、葡萄、马铃薯和观赏植物；2013年8月1日，唑嘧菌胺被列入欧盟农药登记条例已登记有效成分名单，用于葡萄、蔬菜和马铃薯；2013年8 月6日，98％唑嘧菌胺原药在我国获得临时登记；迄今，唑嘧菌胺已在全球50多个国家取得登记。包括葡萄、土豆、西红柿、生菜及其他蔬菜等。唑嘧菌胺具有独特的作用机理，这使其成为此分类中唯一的现有杀菌剂，因此与其他商品化的杀菌剂没有交互抗性，这使唑嘧菌胺成为特种作物上真菌抗性治理的理想工具。
我国GB 2763-2016《食品中农药残留最大限量》中制订了唑嘧菌胺的临时限量，规定了葡萄、黄瓜以及马铃薯中的临时限量分别为2mg/kg、1mg/kg和0.05mg/kg。但是目前还没有制订相应的检测方法。
研发出植物性食品唑嘧菌胺残留量的检测方法，可以满足农产品生产、销售以及监督抽查各环节对于唑嘧菌胺检测的迫切需求，具备比较广泛的市场前景2016年全球登记或上市的新农药有49个。其中巴斯夫在西班牙等级唑嘧菌胺和烯酰吗啉复配农药应用于蔬菜。
目前对于唑嘧菌胺的检测研究集中在农药成分的分析和环境土壤中的含量上，由于含量较高，多采用液相色谱法进行检测分析。比如姜宜飞等2010于《农药科学与管理》发表的“烯酰吗啉.唑嘧菌胺悬浮剂高效液相色谱分析方法研究”，郭子靖等2012年于《农药科学与管理》发表的“土壤中唑嘧菌胺残留超高效液相色谱检测方法研究”等。
对于植物性食品中唑嘧菌胺的残留量的检测，目前研究还比较少。刘磊等2017年《食品安全质量检测学报》发表了“超高效液相色谱-串联质谱法测定辣椒及其栽培土壤中烯酰吗啉和唑嘧菌胺”，辣椒和土壤样品采用乙腈和水提取，盐析后取上清液进行测试，在辣椒和土壤中检出限均可达到10μg/kg。但该法简单的提取盐析后即上液质进行测试，不能适用于基质复杂的各种植物性食品，适用范围小。
Mingfeng Hu等2015年于《Food Chemistry》发表的“Deternination ofametoctradin residue in fruits and vegetables by modified quick，easy，cheap，effective，rugged，and safe method using ultra-performance liquidchromatography/tandem sepcetrometry”。主要针对蔬菜和水果基质，检测唑嘧菌胺。根据苹果、黄瓜等不同的果蔬，尝试了不同的QuChers填料处理样品，去除样品中的色素、糖等干扰物。但是对于其他的样品，比如油脂含量高的粮谷油菜类样品以及基质负责的茶叶类等样品，净化效果并不理想。
A.S.Komarova等2017年于《Journal of Analytical Chemistry》发表了“Determination of ametoctradin in plant residues and environmental samples byHPLC with an UV detector”，土壤和一些植物性食品采用丙酮水溶液提取，固相萃取净化，液相色谱紫外检测器检测，检出限可以达到5-10μg/kg。该法采用固相萃取净化，适用范围广，检出限低。但是采用液相色谱紫外检测器进行检测，容易出现假阳性结果。传统的固相萃取柱，萃取步骤繁琐，耗时长。
因此，发明一种方法前处理步骤简单新颖，净化效果好，回收率高的测定植物性食品中唑嘧菌胺残留量的检测方法十分必要。
发明内容
本发明所要解决的技术问题是适用于植物性食品中唑嘧菌胺残留量的检测方法，能够有效的提取植物性食品中残留的唑嘧菌胺，并很好的去除干扰物。检出限能满足国家标准对糙米、稻谷和苹果中唑嘧菌胺最大残留限量的要求。
本发明的技术方案是通过以下步骤实现的：
(1)提取：
称取均匀样品10g于50ml离心管中，加入30ml甲醇，均质提取，8000r/min冷冻离心后，取上清液，残渣再用20ml甲醇重复提取一次，合并上清液，加入6g无水硫酸镁和150mgN-丙基乙二胺固相吸附剂，震摇，转移上清液至旋蒸瓶中，40℃旋蒸至近干，80％乙腈溶液复溶并定容至5ml，为待净化液；
(2)净化：
将待净化液过Oasis PRiME HLB柱净化；上样过程维持1滴/秒，收集流出液，过0.22μm 滤膜，得样品溶液，供液相色谱串联质谱测定；
(3)测定：
在下述液相色谱串联质谱条件下对标准溶液和试样处理液进行测定：
a.色谱条件：
色谱柱：C18，1.7μm，2.1mm×50mm
流动相：0.1％甲酸溶液(A)+0.1％甲酸乙腈溶液(B)，梯度洗脱，程序为起始流动相比例，0.1％甲酸水溶液；0.1％甲酸乙腈溶液95∶5；2min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；5.5min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液0∶100；6min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液0∶100；7min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；7.5min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；
流速：0.5mL/min；
进样量：5.0μL；
柱温：40℃；
b.质谱条件：
离子源：ESI电喷雾离子源；
扫描方式：正离子扫描；
检测方式：MRM多反应监测；
离子源温度：120℃；
去溶剂温度：450℃
母离子为276.4，定量离子为149.4，定性离子为176.3；
锥孔电压为50V，定量离子碰撞能量为35eV，定性离子对碰撞能量为40eV。
附图说明
图1为10μg/L唑嘧菌胺标准溶液色谱图
具体实施方法
本发明将通过以下实施例作进一步说明。实施例仅用于说明本发明而不用于限制本发明的范围。除非另行定义，文中所使用的所有专业与科学用语与本领域熟练人员所熟悉的意义相同。此外，任何与所记载内容相似或均等的方法及材料皆可用于本发明中，文中所述的较佳实施方法仅作示范之用。
实施例1
1、仪器与试剂
高效液相色谱-串联质谱仪：美国Waters，UPLC-Xevo TQ；
标准物质：唑嘧菌胺，100mg/L；
甲醇：色谱纯；
乙腈：色谱纯；
甲酸：分析纯
无水硫酸镁：分析纯；
Oasis PRiME HLB：6mL，200mg；
本方法中所用水均为一级水。
2、仪器分析条件
a.液相色谱条件：
色谱柱：Waters，BEH C18，1.7μm，2.1mm×50mm
流动相：0.1％甲酸水溶液(A)+0.1％甲酸乙腈溶液(B)，梯度洗脱，程序为起始流动相比例，0.1％甲酸水溶液；0.1％甲酸乙腈溶液95∶5；2min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；5.5min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液0∶100；6min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液0∶100；7min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；7.5min，0.1％甲酸水溶液∶0.1％甲酸乙腈溶液95∶5；
流速：0.3mL/min；
进样量：5.0μL；
柱温：40℃；
b.质谱条件：
离子源：ESI电喷雾离子源；
扫描方式：正离子扫描；
检测方式：MRM多反应监测；
离子源温度：120℃；
去溶剂温度：450℃
母离子为276.4，定量离子为149.4，定性离子为176.3；
锥孔电压为50V，定量离子碰撞能量为35eV，定性离子对碰撞能量为40eV。
3、线性方程
标准储备液配制：称取10mg唑嘧菌胺标准物质，用甲醇溶解并定容至10mL，标准储备液浓度为1000mg/L。
用上述标准溶液配制标准工作液：浓度为0.005mg/L、0.010mg/L、0.020mg/L、0.100 mg/L和0.200mg/L。在上述仪器分析条件下进行测定，外标法定量。以峰面积y为纵坐标，浓度x为横坐标进行线性回归，结果如表1
表1 唑嘧菌胺保留时间，回归方程及线性相关系数
4、样品前处理方法
(1)提取：
称取均匀样品10g于50ml离心管中，加入30ml甲醇，均质提取，8000r/min冷冻离心后，取上清液，残渣再用20ml甲醇重复提取一次，合并上清液，加入6g无水硫酸镁和150mgN-丙基乙二胺固相吸附剂，震摇，转移上清液至旋蒸瓶中，40℃旋蒸至近干，80％乙腈溶液复溶并定容至5ml，为待净化液；
(2)净化：
将待净化液过Oasis PRiME HLB柱净化；上样过程维持1滴/秒，收集流出液，过0.22μm 滤膜，得样品溶液，供液相色谱串联质谱测定；
5、样品测定
称取6份样品，按4所述前处理方法处理样品，按2所述仪器分析条件检测，保留时间、离子丰度比定性，外标法定量。实验结果如表2所示
表2 苹果样品中唑嘧菌胺的测定结果
6、精密度及回收率
本方法的精密度及回收率实验结果如表3所示。
表3 回收率实验结果
7、检出限
唑嘧菌胺检出限为0.3μg/kg，定量限1μg/kg。
Claims (1)
1.一种测定植物性食品中唑嘧菌胺残留量的液相色谱串联质谱法，其特征在于，包括以下步骤：
(1)提取：
称取均匀样品10g于50ml离心管中，加入30ml甲醇，均质提取，8000r/min冷冻离心后，取上清液，残渣再用20ml甲醇重复提取一次，合并上清液，加入6g无水硫酸镁和150mgN-丙基乙二胺固相吸附剂，震摇，转移上清液至旋蒸瓶中，40℃旋蒸至近干，80％乙腈溶液复溶并定容至5ml，为待净化液；
(2)净化：
将待净化液过Oasis PRiME HLB柱净化；上样过程维持1滴/秒，收集流出液，过0.22μm滤膜，得样品溶液，供液相色谱串联质谱测定；
(3)测定：
在下述液相色谱串联质谱条件下对标准溶液和样品溶液进行测定：
a.色谱条件：
色谱柱：C18，1.7μm，2.1mm×50mm；
流动相：A相为0.1％甲酸溶液+B相为0.1％甲酸乙腈溶液，梯度洗脱，程序为起始流动相比例，0.1％甲酸水溶液：0.1％甲酸乙腈溶液95∶5；2min，0.1％甲酸水溶液：0.1％甲酸乙腈溶液95∶5；5.5min，0.1％甲酸水溶液：0.1％甲酸乙腈溶液0∶100；6min，0.1％甲酸水溶液：0.1％甲酸乙腈溶液0∶100；7min，0.1％甲酸水溶液：0.1％甲酸乙腈溶液95∶5；7.5min，0.1％甲酸水溶液：0.1％甲酸乙腈溶液95∶5；
流速：0.5mL/min；
进样量：5.0μL；
柱温：40℃；
b.质谱条件：
离子源：ESI电喷雾离子源；
扫描方式：正离子扫描；
检测方式：MRM多反应监测；
离子源温度：120℃；
去溶剂温度：450℃；
母离子为276.4，定量离子为149.4，定性离子为176.3；
锥孔电压为50V，定量离子碰撞能量为35eV，定性离子对碰撞能量为40eV。
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