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Method for rapidly determining benzo (a) pyrene in edible oil and fat

A technology for rapid determination of edible oils and fats, which is applied to the rapid determination of benzopyrene in edible oils and fats, and based on solid-phase extraction technology for rapid determination of benzopyrene in edible oils and fats in the field of liquid chromatography-tandem mass spectrometry, which can solve the problem of low immunological detection sensitivity , quantitative analysis is not accurate enough, Raman spectroscopy is not mature enough, etc., to achieve the effect of good popularization and application value, less reagent consumption, and improved sensitivity

Pending Publication Date: 2020-10-09
江苏省理化测试中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the low sensitivity and poor thermal stability of GC-MS method, its use is limited in many cases
The qualitative ability of high performance liquid chromatography is not enough; surface-enhanced Raman spectroscopy is not mature enough, its application is less, and the quantitative analysis is not accurate enough; the sensitivity of immunological detection is not high; LC-MS / MS method can improve the sensitivity and qualitative at the same time ability

Method used

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  • Method for rapidly determining benzo (a) pyrene in edible oil and fat
  • Method for rapidly determining benzo (a) pyrene in edible oil and fat
  • Method for rapidly determining benzo (a) pyrene in edible oil and fat

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Experimental program
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Effect test

Embodiment 1

[0041] Embodiment 1: the mensuration of benzo (a) pyrene in liquid edible oil

[0042] (1) Standard curve preparation: Preparation of benzo(a)pyrene standard stock solution: accurately pipette 1mL of 100μg / mL benzo(a)pyrene standard product into a 10mL volumetric flask, dilute to the mark with acetonitrile, and store at -20°C spare. Preparation of internal standard benzo(a)pyrene-D12 standard stock solution: accurately pipette 1mL of 100μg / mL benzo(a)pyrene-D12 standard into a 10mL volumetric flask, dilute to the mark with acetonitrile, and store at -20°C for later use . Take an appropriate amount of benzo(a)pyrene standard stock solution and dilute it step by step to prepare standard working solutions with concentrations of 0.5ng / mL, 1.0ng / mL, 2.0ng / mL, 5.0ng / mL, and 10.0ng / mL.

[0043] (2) Sample pretreatment: Weigh about 0.4 g of liquid edible oil (Fulinmen corn oil, commercially available), add 4 μL of internal standard benzo(a)pyrene-D12 solution with a concentration of...

Embodiment 2

[0051] Embodiment 2: the mensuration of benzo (a) pyrene in solid edible oil and fat

[0052] (1) Standard curve preparation: the operation method is consistent with the method in step (1) of the above-mentioned embodiment 1.

[0053] (2) Sample pretreatment: Weigh about 0.4g of solid oil (butter, Chongqing Shuaike Food Co., Ltd.), add the above oil sample to 1000mg of florisil, stir and mix with a glass rod, and fill it to the Fill it into an extraction column filled with 500 mg C18, add 6 mL of acetonitrile to elute directly, collect all the effluent, concentrate to 0.4 mL, filter through a 0.45 μm organic filter membrane, and analyze by liquid chromatography-tandem mass spectrometer.

[0054] (3) Liquid chromatography-tandem mass spectrometry measurement: the operation steps and chromatographic conditions are consistent with the measurement method in step (3) of the above-mentioned embodiment 1.

[0055] (4) Standard spike recovery and repeatability: select tallow as the m...

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Abstract

The invention discloses a method for rapidly determining benzo (a) pyrene in edible oil and fat. The method comprises steps: after processing a sample based on a solid-phase extraction technology, a sample enters liquid chromatography-tandem mass spectrometry, a composite solid-phase extraction column filled with octadecylsilane chemically bonded silica and florisil filler serves as a purificationtechnology, the influence of factors such as the filler type of the solid-phase extraction column, the filler dosage, an elution solvent and the elution volume on the extraction efficiency is investigated, and liquid chromatography conditions and mass spectrometry conditions are optimized. The method is simple, convenient and rapid to operate and high in accuracy, the detection limit can meet thedetection requirements of benzo (a) pyrene residues in edible oil and fat, the analysis cost is low, and reference can be provided for determination of benzo (a) pyrene in other products.

Description

technical field [0001] The invention belongs to the technical field of food detection, and in particular relates to a method for rapidly determining benzo(a)pyrene in edible oils and fats, in particular to a method for rapidly determining benzo(a)pyrene in edible oils and fats based on solid-phase extraction technology. The method of tandem mass spectrometry. Background technique [0002] Benzo(a)pyrene, referred to as Bap, also known as 3,4-benzopyrene, is a polycyclic aromatic hydrocarbon composed of five benzene rings. Benzo(a)pyrene is a strong carcinogen, which is produced by the polymerization of organic compounds under high temperature conditions. Edible oil itself does not contain or contains very little benzo(a)pyrene, but it is produced during planting and processing. , transportation and cooking process, it is often contaminated, and the difficulty in the detection of benzo(a)pyrene in edible oils and fats lies in the removal of lipid interference. At present, n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/72
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N2030/045G01N2030/062G01N2030/146
Inventor 朱成晶高宏郭芳芳徐慧贾涛
Owner 江苏省理化测试中心
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