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Method for analyzing and detecting a plurality of endocrine disruptors in food

An endocrine disruptor and food technology, applied in the field of food inspection, can solve the problems of high solvent consumption, high sensitivity, inability to take into account structural interpretation and sensitivity, etc., and achieve the effect of accurate analysis and improved sensitivity

Active Publication Date: 2013-07-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when progesterone, androgen, estrogen and phenols need to be analyzed at the same time in the research, they are divided into two groups, namely progesterone, androgen, estrogen and phenols, and are determined twice according to the above analysis method , which is time-consuming and solvent-intensive
[0004] In the quantitative analysis of the triple quadrupole, the multiple reaction monitoring mode is usually used to obtain higher sensitivity. However, in this mode, the fragment ion information used for structural interpretation other than the detected ions is discarded; while in the ion full scan mode , and a greater loss of sensitivity
The quadrupole time-of-flight mass spectrometer can obtain the accurate molecular weight of all fragment ions with high sensitivity, which overcomes the dilemma that the triple quadrupole cannot take into account the structural interpretation and sensitivity
However, in the analysis of food endocrine disruptors, because the content of endocrine disruptors is often extremely low (ng / kg or pg / kg level), this concentration level is close to the detection limit of quadrupole time-of-flight mass spectrometer, and quadrupole Time-of-Flight Mass Spectrometry Difficult to Accurately Analyze Endocrine Disruptors in Food

Method used

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  • Method for analyzing and detecting a plurality of endocrine disruptors in food
  • Method for analyzing and detecting a plurality of endocrine disruptors in food
  • Method for analyzing and detecting a plurality of endocrine disruptors in food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Determination of 26 endocrine disruptors in milk powder

[0033] 1. Instruments and reagents:

[0034] ACQUITY ultra-high performance liquid chromatography (Waters, USA), SYNAPT G2 high-resolution time-of-flight mass spectrometer (Waters, USA), 2200T ultrasonic cleaner (Shanghai Anpu), TGL-10B high-speed desktop centrifuge (Shanghai Anting), KD200 Nitrogen purging instrument (Hangzhou Aosheng); 12-position solid phase extraction apparatus (Germany CNW); C18 solid phase extraction column (Shanghai Dima, 500mg, 3mL); LC-MS grade acetonitrile (U.S. Fisher), LC-MS grade Pure water (Fisher, USA), LC-MS grade ethyl acetate (Fisher, USA), superior pure sodium chloride (Shanghai Sinopharm Group).

[0035]Standard products: 10 estrogens, 7 progestins and 3 phenols were purchased from Sigma in the United States, and 6 androgens were purchased from Dr. Ehrenstorfer in Germany; the purity of the standard products was greater than 97.8%. Preparation of standard stock sol...

Embodiment 2

[0054] Example 2 Determination of 26 endocrine disruptors in pure milk

[0055] 1, the apparatus and reagents are the same as in Example 1.

[0056] 2. Analysis method: In the sample pretreatment, "take 10mL of the mixed milk sample, put it in a 50mL plastic centrifuge tube with a stopper, add 20mL of acetonitrile, shake for 2min, and ultrasonically extract for 10min..." It is different from Example 1 , the rest of the steps are the same as in Example 1.

[0057] 3. Results of Sample Determination

[0058] The method of the present invention is used to analyze and measure 3 parts of whole milk of 3 common different brands purchased, and the results show that progesterone and androstenedione are detected in the 3 parts of milk samples, and the concentrations are respectively 8.1-12.7 μg / L ( 10.1 μg / L on average) and 0.39-0.79 μg / L (0.61 μg / L on average).

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Abstract

The invention belongs to the field of food inspection, relates to an assay determination method for endocrine disruptors in food, and particularly relates to a method for analyzing and determining a plurality of endocrine disruptors in milk powder and liquid milk. The method comprises the steps of dissolving a sample with water, adding an organic solvent mixable with water, extracting a to-be-detected material by ultrasonic, adding a sodium salt to make the organic solvent separated from a water phase to realize liquid-liquid extraction, taking an organic solvent containing quantitative to-be-detected material, purifying by extraction with a solid phase filled with C 18 materials, deriving by dansyl chloride, and analyzing and detecting four types of 26 endocrine disruptors in the food by using ultra-high performance liquid chromatography-quadrupole-time of flight-mass spectrometry at the same time. The method can overcome the disadvantages that a conventional technology cannot realize simultaneous analysis of the plurality of the endocrine disruptors in the food by once chromatographic sample injection, can increase sensitivity of the quadrupole-time of the flight-mass spectrometry, and realize accurate analysis of the endocrine disruptors in the food by using the quadrupole-time of the flight-mass spectrometry.

Description

technical field [0001] The invention belongs to the field of food inspection, and relates to a method for analyzing and measuring food endocrine disruptors, in particular to a method for analyzing and measuring various endocrine disruptors in milk powder and liquid milk. In particular, the solid phase extraction-ultra-high performance liquid chromatography tandem quadrupole time-of-flight mass spectrometry method is used to simultaneously analyze 26 kinds of 4 types of endocrine disruptors in milk powder and liquid milk. Background technique [0002] Studies have shown that endocrine disruptors can interfere with the endocrine system, and those that cause harmful effects to animals or humans are often natural or compounds related to human activities. Exposure to endocrine disruptors has been reported in the literature to be associated with precocious puberty, prostate cancer, uterine cancer, and breast cancer, among other hormone-related diseases. Food is an important route...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 王和兴周颖姜庆五
Owner FUDAN UNIV
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