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Method for detecting nine cholesterol oxides in food by gas chromatography-mass spectrometry

A cholesterol oxide and gas chromatography technology is applied in the field of cholesterol oxide detection to achieve the effects of improving accuracy, good repeatability and satisfactory recovery rate

Active Publication Date: 2021-08-24
深圳深检集团医学检验实验室
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Problems solved by technology

[0004] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for detecting 9 kinds of cholesterol oxides in food by gas chromatography-mass spectrometry, which solves the problem of the limitation in the detection of cholesterol oxides in complex samples in the prior art, and has the advantages of Accurate and efficient, high detection limit, high sensitivity, and good repeatability

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  • Method for detecting nine cholesterol oxides in food by gas chromatography-mass spectrometry
  • Method for detecting nine cholesterol oxides in food by gas chromatography-mass spectrometry
  • Method for detecting nine cholesterol oxides in food by gas chromatography-mass spectrometry

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Embodiment

[0054] EXAMPLES: This example is to obtain a compounding experiment for the food product to verify the feasibility of the method of the present invention, and processed according to the following steps:

[0055] S1: Choose fresh fish, pork and beef samples, uniformly crush, as blank samples, accurately weigh 2.0 g of samples in the triangular bottle, add high, medium, low 3 horizontal concentrations of COPS series mixed standard working fluid . The 150 ml of volume ratio of 2: 1 is 2: 1, methanol is an extract, which is fully oscillated for 2min, then ultrasonically 30min; in the 4 ° C environment overnight, stand in a layer, then filter paper, to dry the filtrate, nitrogen Get a lipid extract;

[0056] S2: Saponification: Add 10 ml of 1 mol / L of KOH solution, 10 ml of methanol, sufficiently oscillating, ultrasonic extract, and completely dissolve the lipid extract, and then freeze the soap for 10 h at room temperature. Deion water transferred to a separatory funnel, and then re...

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Abstract

The invention relates to a method for detecting nine cholesterol oxides in food by gas chromatography-mass spectrometry, which comprises the following steps: S1, adding 19-hydroxycholesterol as an internal standard substance to carry out sample lipid extraction; S2, dissolving the obtained lipid extract, and carrying out saponification extraction to remove moisture so as to obtain a concentrated filtrate; S3, purification and concentration: adding 3mL of n-hexane, shaking and dissolving, adding into activated NH2-SPE, washing the column, discarding waste liquid, collecting filtrate, and blow-drying by nitrogen; S4, derivatization: adding 100 [mu] L of N, O-bis (trimethylsilane) trifluoroacetamide BSTFA for derivatization for 40 min, blow-drying with nitrogen, and dissolving with 1.0 mL of n-hexane to a constant volume; and S5, taking a mixed standard solution of nine cholesterol oxides, detecting the mixed standard solution under gas chromatography conditions and mass spectrometry conditions, and drawing a standard curve. According to the method, a pretreatment mode suitable for complex samples is established, saponification conditions and a solid-phase extraction column are optimized, the accuracy of analysis and detection is improved by adopting an internal standard substance, and the method has the advantages of accuracy, high efficiency and wide applicability.

Description

Technical field [0001] The present invention relates to the field of cholesterol oxide detection techniques, and more particularly to methods of detecting nine cholesterol oxides in foods in gas chromatography - mass spectrometry. Background technique [0002] Cholesterol Oxidation Products, COPS is an oxidative product of cholesterol, generally in meat products, dairy products, egg products and animal fats. During the production process and treatment of food, cholesterol is prone to its own oxidation reaction by light, oxygen and high temperatures, etc., and is derived from cholesterol oxidation products. [0003] Medical studies have shown that foodborne cholesterol oxides will cause certain damage to health. Studies have pointed out that cholesterol oxides and human atherosclerosis, cytotoxic effects, gene mutation, and even carcinogenic relationships. Cholesterol oxides have become a new hot spot for food safety, but the cholesterol oxide in food is still difficult to conduct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 杨俊吴轩民张协光
Owner 深圳深检集团医学检验实验室
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