CN107843477A - 食品中苯并[a]芘的快速提取方法 - Google Patents

食品中苯并[a]芘的快速提取方法 Download PDF

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CN107843477A
CN107843477A CN201710918439.6A CN201710918439A CN107843477A CN 107843477 A CN107843477 A CN 107843477A CN 201710918439 A CN201710918439 A CN 201710918439A CN 107843477 A CN107843477 A CN 107843477A
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food
pyrene
benzo
filter membrane
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谈义萌
唐涛
杨三东
夏明珠
王风云
李彤
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YILITE ANALYSIS INSTRUMENT CO Ltd DALIAN
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids
    • B01D11/0215—Solid material in other stationary receptacles
    • B01D11/0223—Moving bed of solid material
    • B01D11/0238—Moving bed of solid material on fixed or rotating flat surfaces, e.g. tables combined with rotating elements or on rotating flat surfaces
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material

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Abstract

本发明公开一种食品中苯并[a]芘的快速提取方法，按照如下步骤：将食品烘干后用均质分散器粉碎并均质化，得样品备用；向离心管中依次加入A组分、B组分及蒸馏水，混合均匀后3000~8000r/min离心3~10min，使超分子溶剂相与水相上下分层，移除下层水相，保留上层超分子溶剂；A组分、B组分及蒸馏水的质量比为1：0.2~0.4：5~10；A组分为四丁基氢氧化铵、四丁基溴化铵、四丁基硫酸氢铵中的至少一种，B组分为庚醇、辛醇、壬醇中的至少一种；将步骤a所得样品与步骤b所得超分子溶剂混合并在常温下以20~40KHz超声处理5~20min，然后将混合液过0.45μm有机滤膜，取过滤膜液体。

Description

食品中苯并[a]芘的快速提取方法
技术领域
本发明涉及一种食品检测技术，尤其是一种省时省力、操作简便、环境友好的食品中苯并[a]芘的快速提取方法。
背景技术
苯并[a]芘是多环芳烃类化合物中的一种具有明显致癌作用的有机化合物，在高温烹调的食品中容易产生，研究表明，苯并[a]芘可致肺癌、肝癌、肠胃道癌症等，属于一级致癌物。近年来，苯并[a]芘所造成的食品安全问题也日益受到人们的重视，我国国标限定粮食和肉制品中苯并[a]芘的残留量应在5μg/kg以下，植物油中为10μg/kg以下。目前，食品中苯并[a]芘含量的测定方法主要有荧光光度法、酶联免疫吸附法、气相色谱－质谱联用法和高效液相色谱法，而大多测量方法需要在检测前对被测食品进行提取处理。现有食品中苯并[a]芘的提取方法为固相萃取，即采用固相萃取小柱对样品进行净化，以提取食品中的苯并[a]芘，存在着操作繁琐、有机溶剂量大、耗时长等缺点，样品多时则无法满足检测的要求。
发明内容
本发明是为了解决现有技术所存在的上述技术问题，提供一种省时省力、操作简便、环境友好的食品中苯并[a]芘的快速提取方法。
本发明的技术解决方案是：一种食品中苯并[a]芘的快速提取方法，其特征在于按照如下步骤进行：
a. 将食品烘干后用均质分散器粉碎并均质化，得样品备用；
b. 向离心管中依次加入A组分、B组分及蒸馏水，混合均匀后3000~8000r/min离心3~10min，使超分子溶剂相与水相上下分层，移除下层水相，保留上层超分子溶剂在密封瓶中；所述A组分、B组分及蒸馏水的质量比为1：0.2~0.4：5~10；所述A组分为四丁基氢氧化铵、四丁基溴化铵、四丁基硫酸氢铵中的至少一种，所述B组分为庚醇、辛醇、壬醇中的至少一种；
c. 将步骤a所得样品与步骤b所得超分子溶剂混合，样品量与溶剂用量比为1g：1~5mL，在常温下以20~40KHz超声处理5~20min，然后将混合液过0.45 μm有机滤膜，取过滤膜液体。
本发明是利用超分子溶剂萃取食品中的苯并[a]芘，萃取剂可直接进样分析，无需进一步蒸发或净化步骤，整个样品处理过程只需大约30分钟，可同时处理多个样品。本发明的检出限（S/N≥3）为0.11μg/kg，在0.1~50μg/kg浓度范围内线性相关系数R2=0.9999。具有操作简单快速、溶剂用量少、安全环保、萃取效率高且稳定，有利于食品中苯并[a]芘的准确快速的定性定量检测。
附图说明
图1是本发明实施例1中方便面基质加标10.0 µg/kg谱图。
具体实施方式
实施例1：
a. 将方便面烘干后用均质分散器粉碎并均质化，得样品备用；
b. 向10ml离心管中依次加入300 mg四丁基溴化铵、100mg辛醇和8 mL蒸馏水，混合均匀后8000r/min离心3min，使超分子溶剂相与水相上下分层，用注射器移除下层水相，将上层超分子溶剂保存在密封瓶中；
c. 取200 mg步骤a所得样品与800 µL步骤b所得超分子溶剂混合并在常温下以20KHz超声处理10min，然后将混合液过0.45 μm有机滤膜，取过滤膜液体。
实施例2：
a. 将油条烘干后用均质分散器粉碎并均质化，得样品备用；
b. 向10ml离心管中依次加入300 mg四丁基氢氧化铵、100mg庚醇和8 mL蒸馏水，混合均匀后5000r/min离心8min，使超分子溶剂相与水相上下分层，用注射器移除下层水相，将上层超分子溶剂保存在密封瓶中；
c. 取400 mg步骤a所得样品与1000 µL步骤b所得超分子溶剂混合并在常温下以40KHz超声处理5min，然后将混合液过0.45 μm有机滤膜，取过滤膜液体。
实验：
分别取实施例1、2所得样品10 μL进行液相色谱分析。液相色谱分析条件如下：流动相为乙腈/水=80/20（v/v），流速为1.0 mL/min；荧光检测器的检测波长设为激发波长=290nm，发射波长=410 nm；柱温为35℃。
测定结果如下表：
本发明实施例1中方便面基质加标10.0 µg/kg谱图如图1所示。

Claims (1)

1.一种食品中苯并[a]芘的快速提取方法，其特征在于按照如下步骤进行：
a. 将食品烘干后用均质分散器粉碎并均质化，得样品备用；
b. 向离心管中依次加入A组分、B组分及蒸馏水，混合均匀后3000~8000r/min离心3~10min，使超分子溶剂相与水相上下分层，移除下层水相，保留上层超分子溶剂在密封瓶中；所述A组分、B组分及蒸馏水的质量比为1：0.2~0.4：5~10；所述A组分为四丁基氢氧化铵、四丁基溴化铵、四丁基硫酸氢铵中的至少一种，所述B组分为庚醇、辛醇、壬醇中的至少一种；
c. 将步骤a所得样品与步骤b所得超分子溶剂混合，样品量与溶剂用量比为1g：1~5mL，在常温下以20~40KHz超声处理5~20min，然后将混合液过0.45 μm有机滤膜，取过滤膜液体。
CN201710918439.6A 2017-09-30 2017-09-30 食品中苯并[a]芘的快速提取方法 Withdrawn CN107843477A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111665313A (zh) * 2020-07-03 2020-09-15 孟祥龙 一种水产品中多氯联苯类化合物的测定方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104391055A (zh) * 2014-11-17 2015-03-04 深圳市宇驰检测技术有限公司 一种检测、分析粮食中苯并[a]芘的方法
CN105017465A (zh) * 2015-08-14 2015-11-04 云南健阳科技有限公司 苯并(a)芘磁性碳纳米管表面分子印迹聚合物及其用途

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104391055A (zh) * 2014-11-17 2015-03-04 深圳市宇驰检测技术有限公司 一种检测、分析粮食中苯并[a]芘的方法
CN105017465A (zh) * 2015-08-14 2015-11-04 云南健阳科技有限公司 苯并(a)芘磁性碳纳米管表面分子印迹聚合物及其用途

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
ANA BALLESTEROS-GÓMEZ ET AL.: "Environment-Responsive Alkanol-Based Supramolecular Solvents: Characterization and Potential as Restricted Access Property and Mixed-Mode Extractants", 《ANALYTICAL CHEMISTRY》 *
FRANCISCO JOSÉ LÓPEZ-JIMÉNEZ ET AL.: "Determination of polycyclic aromatic hydrocarbons (PAH4) in food by vesicular supramolecular solvent-based microextraction and LC-fluorescence detection", 《FOOD CHEMISTRY》 *
MORTEZA MORADI ET AL.: "Ultrasound-assisted liquid-phase microextraction based on a nanostructured supramolecular solvent", 《ANAL BIOANAL CHEM》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111665313A (zh) * 2020-07-03 2020-09-15 孟祥龙 一种水产品中多氯联苯类化合物的测定方法

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Application publication date: 20180327