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Method for determining three typical quaternary ammonium compounds in overground part of plant

A quaternary ammonium salt compound, aboveground technology, applied in the field of detection, can solve the problems of thermal decomposition of BACs, massive dissolution of pigment impurities, inability to achieve accurate quantification, etc.

Active Publication Date: 2020-10-23
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the detection method of QACs in plants is mainly aimed at QACs of a single structure type, and there is no report on the detection method of QACs applicable to three structure types at the same time.
Some methods for ATMACs and DADMACs use gas chromatography-mass spectrometry as a quantitative analysis instrument, but this type of instrument may cause thermal decomposition of BACs during the analysis process, making accurate quantification impossible
In addition, the use of polar organic solvents in the process of extracting plant shoot samples will lead to a large amount of elution of pigment impurities, which will interfere with the quantitative analysis on the instrument in the later stage

Method used

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  • Method for determining three typical quaternary ammonium compounds in overground part of plant
  • Method for determining three typical quaternary ammonium compounds in overground part of plant
  • Method for determining three typical quaternary ammonium compounds in overground part of plant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of embodiment of the method for measuring three kinds of typical quaternary ammonium salt compounds in the shoot of plant described in the present invention, the method described in the present embodiment comprises the following steps:

[0031] (1) Sample pretreatment process: freeze-dry the plant sample and grind it to powder;

[0032] (2) Sample extraction process: Accurately weigh 0.1g of plant shoot samples into a 50mL Teflon centrifuge tube, add 10μL recovery rate indicator TBAC-d7 (concentration is 1.0μg mL -1 ) and 15mL extract (methanol extract containing 0.1% hydrochloric acid (v / v)), shake a few times, ultrasonically extract for 20 minutes, centrifuge (13000rpm, 20min), repeat three times, and combine the supernatant into a 100mL chicken heart bottle , concentrated by rotary evaporation to less than 1mL to obtain an extract;

[0033] (3) Purification process: pass the extract of the aboveground sample of the plant through the CNWBOND Alumina-N SPE extr...

Embodiment 2

[0043] Optimization of purification process for samples of aboveground parts of plants

[0044] In order to reduce the interference of the pigment dissolved in the above-ground part of the plant on the subsequent detection, the above-ground part of wheat was used as the representative of the above-ground part of the test plant, and the recovery experiment of different concentrations of QACs was carried out to investigate the effect of different leaching methods on reducing the pigment. pros and cons. In this method, three treatment methods were compared, namely no rinsing, rinsing with ethyl acetate and rinsing with a mixed solution of isobutanol / n-hexane (1:1, v / v). Specific steps are as follows:

[0045] (1) Select an uncontaminated wheat aerial part sample (i.e. a blank matrix sample of the plant aerial part), grind it for subsequent use after freeze-drying;

[0046] (2) Carry out the pretreatment according to the step (2) of Example 1 to obtain the blank matrix extract o...

Embodiment 3

[0051] Verification of the applicability of the method of the present invention

[0052] Taking the aboveground part of wheat as the representative of the aboveground part of the tested plants, the applicability of this method was investigated by carrying out spike recovery experiments of different concentrations of QACs. Specific steps are as follows:

[0053] (1) Dilute the QACs standard stock solution (μg mL) with 60% aqueous methanol -1 ), prepare three samples of QACs (0.2, 0.4, 0.6, 0.8, 1, 2, 4, 6, 8, 10μg L -1 ), measured by LC-MS / MS according to Example 1 step (4), carried out quantitative analysis with internal standard method, and calculated the marking lines of three kinds of QACs by linear regression. The instrument detection limits (Instrument detection limits, IDLs) of the three QACs were calculated based on the 3-fold signal-to-noise ratio of the QACs for low-concentration samples, while the method detection limits (Method detection limits, MDLs) were calcula...

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Abstract

The invention discloses a method for determining three typical quaternary ammonium compounds (dodecyl trimethyl ammonium chloride, dodecyl dimethyl benzyl ammonium chloride and didodecyl dimethyl ammonium chloride) in an overground part of a plant. The method comprises the following steps of: carrying out freeze drying and grinding on a plant overground part sample, adding a recovery rate indicator deuterated tetradecyl dimethyl benzyl ammonium chloride and an extracting agent, and carrying out ultrasonic extraction to obtain an extract solution; purifying the extract solution through a neutral aluminum oxide solid-phase extraction column; adding an internal standard substance tetrabutylammonium nitrate into the purified extract solution to obtain an extracted purified solution; and performing detection by adopting liquid chromatography-tandem mass spectrometry, performing comparing with three quaternary ammonium compound standard substances which are operated in parallel, determiningthe nature by using retention time and optimized characteristic ions, taking ions with high signal-to-noise ratio, good peak shape and small interference as quantitative ions, and performing quantifying by using an internal standard method. The method is suitable for determining the content of three typical quaternary ammonium compounds in a complex matrix of the overground part of the plant, theresult is accurate, and the recovery rate is high.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for determining three typical quaternary ammonium salt compounds in the aboveground parts of plants. Background technique [0002] Quaternary ammonium compounds (QACs) are a new class of environmental pollutants that have attracted the attention of scholars and the public at home and abroad in the past decade. The quaternary ammonium salt compound is formed by replacing the hydrogen atom of the ammonium root with an alkane or an aromatic hydrocarbon group, and the general formula is (R 4 N + )X - , where R is an alkane or aromatic hydrocarbon group, X - for halide ions. Common QACs can be divided into alkyltrimethylammonium compounds (ATMACs), dialkyldimethylammonium compounds (DADMACs), benzylalkyldimethylammonium salts (Alkyltrimethylammonium compounds, DADMACs) Ammonium salts (Benzylalkyldimethylammonium compounds, BACs), etc. Studies have shown that QACs can produce toxic ...

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
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N2030/062
Inventor 林庆祺李雅菲王诗忠仇荣亮黄雄飞
Owner SUN YAT SEN UNIV
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