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Method for detecting perchlorate in tea leaves by adopting solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

A high-performance liquid chromatography and perchlorate technology, which is applied in the field of solid-phase extraction-high-performance liquid chromatography-tandem mass spectrometry detection of perchlorate in tea, can solve the problems of high price and difficult availability of internal isotope standards, and achieve sensitivity High, good effect, fast analysis effect

Active Publication Date: 2017-10-13
TEA RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although LC-MS / MS is more versatile than IC-MS / MS, isotopic internal standards are expensive and difficult to obtain

Method used

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  • Method for detecting perchlorate in tea leaves by adopting solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting perchlorate in tea leaves by adopting solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
  • Method for detecting perchlorate in tea leaves by adopting solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0022] Example 1: Establishment of Mass Spectrometry Conditions

[0023] Precursor ion of perchlorate obtained by full scan m / z 99, 101, corresponding to 35 ClO 4 - , 37 ClO 4 - , its ion abundance ratio is 3:1, which is the same as the isotope abundance ratio of chloride ion ( 35 Cl: 37 Cl=3:1). Using the above two ions as precursor ions, the optimal declustering voltage of 2 V was obtained; the collision energy was applied to obtain the characteristic product ions respectively m / z 83, 85 and the optimal collision energy 100 V, and the product ion abundance ratio m / z 83:85 is close to 3:1. Select the ion with high abundance m / z 99 > 83 ion channels as quantitative ion pairs, m / z 101 > 85 as qualifier transitions. Mass Spectrum See figure 1 .

Embodiment 2

[0024] Embodiment two: the establishment of liquid phase condition

[0025] Perchlorate is a hydrophilic and strongly polar compound, which has weak retention on reversed-phase chromatographic columns such as C18 and elutes at dead time. The invention compares the retention of perchlorate between the hydrophilic chromatographic column and the graphitized carbon chromatographic column. The retention time of perchlorate on the CORTECS UPLCHILIC (2.1 x 100 mm, 1.6 μm) column was 0.97 min, but it was difficult to achieve baseline separation from the impurities in the tea extract (1.36 min) ( figure 1 ). Adjusting the mobile phase did not effectively separate perchlorate from impurities while improving retention behavior. Perchlorate has a strong retention ability on Thermo Hypercarb column (2.1 x 100 mm, 5 μm), and the retention time of different buffer salt systems is different, ranging from 1.76 min to 10.1 min. The mobile phase was 0.1% formic acid methanol:10 mM ammonium a...

Embodiment 3

[0026] Embodiment three: optimization of extraction solvent

[0027] Literature research finds that acid is often used to assist the extraction of perchlorate. The present invention investigates 0.2% acetic acid aqueous solution, 0.1% formic acid methanol, and utilizes the same solid phase extraction column (such as C18, Cleannert TPT, Cleanert pesti-carb SPE, HLB, Cleanert PWAX) were purified and analyzed by UPLC-MS / MS, and it was found that the extraction effect of 0.2% acetic acid water was better.

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Abstract

The invention discloses a method for detecting perchlorate in tea leaves by adopting solid phase extraction-high performance liquid chromatography-tandem mass spectrometry, and belongs to the field of analysis and detection. According to the method disclosed by the invention, by combining acetic acid aqueous extraction and weak anion exchanged solid phase extraction column purification with a high performance liquid chromatography-tandem mass spectrometry detection technology, the contents of the perchlorate in the tea leaves are separated and analyzed; the method has the advantages of high purification degree of matrix, high sensitivity and accurate qualitation and quantitation. According to the method for detecting the perchlorate in the tea leaves, the recycling rate of the perchlorate in the tea leaves is 97.8 to 101.8 percent, the relative standard deviation is less than 10.0 percent, and the minimum quantification limit is 0.01mg / kg; the method can be used for detecting the perchlorate in the tea leaves.

Description

technical field [0001] The invention belongs to the technical field of detection, and in particular relates to a method for detecting perchlorate in tea by solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] Perchlorate has high water solubility, good stability, weak adsorption on soil and minerals, and easy diffusion. It is a persistent pollutant. Over the years, perchlorate has been produced in large quantities and widely used in rocket propellants, fireworks manufacturing, and the munitions industry. In 1997, perchlorate was detected in water for the first time; subsequently, perchlorate pollution was also found in milk, vegetables, fruits and other foods, which aroused widespread concern. Because perchlorate interferes with the absorption of iodide ions by the human thyroid gland, it affects the synthesis of thyroid hormones, thereby hindering the development of the central nervous system in children, and...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 孙荷芝刘岩陈宗懋
Owner TEA RES INST CHINESE ACAD OF AGRI SCI
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