CN108680668A - 一种食品中多环芳香烃的测定方法 - Google Patents

一种食品中多环芳香烃的测定方法 Download PDF

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CN108680668A
CN108680668A CN201810432180.9A CN201810432180A CN108680668A CN 108680668 A CN108680668 A CN 108680668A CN 201810432180 A CN201810432180 A CN 201810432180A CN 108680668 A CN108680668 A CN 108680668A
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pah
aromatic hydrocarbons
polycyclic aromatic
tandem mass
food
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陈卫东
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Jiangsu Anshun Technical Service Co Ltd
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Jiangsu Anshun Technical Service Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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Abstract

本发明公开了一种食品中多环芳香烃的测定方法，采用气相色谱串联质谱法，包括以下步骤：称取样品，加入丙酮5‑20mL，充分涡旋2min，振荡过夜，离心，取上清液，待净化，取已活化GCB小柱，加入上述上清液，最后用3‑10mL丙酮洗脱，洗脱液氮吹干，用1mL丙酮定容，过膜，上机测试。本发明更加方便的测定出食品中多环芳香烃。

Description

一种食品中多环芳香烃的测定方法
技术领域
本发明涉及一种测定方法，特别涉及一种食品中多环芳香烃的测定方法。
背景技术
现有的国家标准暂时没有对食品中多环芳香烃的测定方法，而食品中具有16种左右的多环芳香烃，通过现有类似的方法进行测定时，其操作比较复杂，耗时长，成本较高。
发明内容
为解决上述背景技术中存在的问题，本发明的目的在于提供一种食品中多环芳香烃的测定方法，以达到更加方便的测定出食品中多环芳香烃的目的。
为达到上述目的，本发明的技术方案如下：
一种食品中多环芳香烃的测定方法，采用气相色谱串联质谱法，其特征在于，包括以下步骤：
称取样品，加入丙酮5-20mL，充分涡旋2min，振荡过夜，离心，取上清液，待净化，取已活化GCB小柱，加入上述上清液，最后用3-10mL丙酮洗脱，洗脱液氮吹干，用1mL丙酮定容，过膜，上机测试。
优选的，所述气相色谱串联质谱法中的气相色谱串联质谱仪的色谱柱为 HP-5MS，载气为高纯氦气99.999％。
优选的，所述气相色谱串联质谱仪的离子源为EI+，进样口温度为280℃，流速为1.0ml/min，进样量为1ul，传输线温度为280℃，离子源温度为 300℃，四极杆温度为180℃，保留时间为甲基毒死蜱18.336min。
优选的，所述气相色谱串联质谱仪的升温程序为100℃保持1min，35℃ /min升至180℃，保持1min，5℃/min升至220℃，保持1min，3℃/min升至280℃，保持0min，30℃/min升至305℃，保持1min。
通过上述技术方案，本发明提供的一种食品中多环芳香烃的测定方法，利用丙酮提取目标物质，固相萃取柱净化后，GC-MS进行测试，可以更加方便的测定食品中16种左右的多环芳香烃，其方法操作简便，耗时短，且节约成本。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述。
本发明提供的一种食品中多环芳香烃的测定方法，一种食品中多环芳香烃的测定方法，采用气相色谱串联质谱法，其特征在于，包括以下步骤：
称取样品，加入丙酮5-20mL，充分涡旋2min，振荡过夜，离心，取上清液，待净化，取已活化GCB小柱，加入上述上清液，最后用3-10mL丙酮洗脱，洗脱液氮吹干，用1mL丙酮定容，过膜，上机测试。
优选的，所述气相色谱串联质谱法中的气相色谱串联质谱仪的色谱柱为 HP-5MS，载气为高纯氦气99.999％。
优选的，所述气相色谱串联质谱仪的离子源为EI+，进样口温度为280℃，流速为1.0ml/min，进样量为1ul，传输线温度为280℃，离子源温度为 300℃，四极杆温度为180℃，保留时间为甲基毒死蜱18.336min。
优选的，所述气相色谱串联质谱仪的升温程序为100℃保持1min，35℃ /min升至180℃，保持1min，5℃/min升至220℃，保持1min，3℃/min升至280℃，保持0min，30℃/min升至305℃，保持1min，参见表1为质谱仪条件表：
表1：
本发明公开的一种食品中多环芳香烃的测定方法，利用丙酮提取目标物质，固相萃取柱净化后，GC-MS进行测试，可以更加方便的测定食品中16种左右的多环芳香烃，其方法操作简便，耗时短，且节约成本。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (4)

1.一种食品中多环芳香烃的测定方法，采用气相色谱串联质谱法，其特征在于，包括以下步骤：
称取样品，加入丙酮5-20mL，充分涡旋2min，振荡过夜，离心，取上清液，待净化，取已活化GCB小柱，加入上述上清液，最后用3-10mL丙酮洗脱，洗脱液氮吹干，用1mL丙酮定容，过膜，上机测试。
2.根据权利要求1所述的一种食品中多环芳香烃的测定方法，其特征在于，所述气相色谱串联质谱法中的气相色谱串联质谱仪的色谱柱为HP-5MS，载气为高纯氦气99.999％。
3.根据权利要求2所述的一种食品中多环芳香烃的测定方法，其特征在于，所述气相色谱串联质谱仪的离子源为EI+，进样口温度为280℃，流速为1.0ml/min，进样量为1ul，传输线温度为280℃，离子源温度为300℃，四极杆温度为180℃，保留时间为甲基毒死蜱18.336min。
4.根据权利要求3所述的一种食品中多环芳香烃的测定方法，其特征在于，所述气相色谱串联质谱仪的升温程序为100℃保持1min，35℃/min升至180℃，保持1min，5℃/min升至220℃，保持1min，3℃/min升至280℃，保持0min，30℃/min升至305℃，保持1min。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010249647A (ja) * 2009-04-15 2010-11-04 Isuzu Motors Ltd 多環芳香族炭化水素類の回収率評価方法
CN104165956A (zh) * 2014-08-14 2014-11-26 同济大学 一种拆迁废物中有机物的测定方法
CN104535665A (zh) * 2014-07-31 2015-04-22 甘肃中天药业有限责任公司 一种党参药材的检测方法
CN104569193A (zh) * 2014-12-29 2015-04-29 山东龙大粮油有限公司 一种食用油中多环芳烃的检测方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010249647A (ja) * 2009-04-15 2010-11-04 Isuzu Motors Ltd 多環芳香族炭化水素類の回収率評価方法
CN104535665A (zh) * 2014-07-31 2015-04-22 甘肃中天药业有限责任公司 一种党参药材的检测方法
CN104165956A (zh) * 2014-08-14 2014-11-26 同济大学 一种拆迁废物中有机物的测定方法
CN104569193A (zh) * 2014-12-29 2015-04-29 山东龙大粮油有限公司 一种食用油中多环芳烃的检测方法

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
杨左军 等: "气相色谱-串联质谱法同时测定纸质食品接触材料中多环芳烃", 《中国造纸》 *
王娟 等: "紫菜中有机氯农药和多环芳烃的气相色谱-质谱联用测定法", 《环境与健康杂志》 *
王敬 等: "固相萃取-气相色谱-串联质谱法测定蔬菜中的16种多环芳烃", 《食品安全质量检测学报》 *
裴德君 等: "气相色谱一质谱联用法同时测定纺织品中的8种多环芳烃", 《分析测试学报》 *

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CN108680668A (zh) 一种食品中多环芳香烃的测定方法

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Application publication date: 20181019