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Method for detecting SUHs in traditional Chinese medicinal materials

A detection method and a technology of traditional Chinese medicinal materials, which are applied in the direction of measuring devices, material separation, and analysis of materials, etc., can solve the problems of cumbersome and time-consuming operations, poor sensitivity and selectivity of SUHs, and low concentration of SUHs, so as to avoid a large amount of use and improve the efficiency of pretreatment , High detection efficiency

Pending Publication Date: 2022-05-13
NINGXIA MEDICAL UNIV
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  • Description
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Problems solved by technology

[0006] Based on this, the present invention provides a method for detecting SUHs in Chinese medicinal materials to solve the technical problems of low SUHs concentration in samples, poor sensitivity and selectivity of SUHs detection, and cumbersome and time-consuming operations in the prior art.

Method used

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  • Method for detecting SUHs in traditional Chinese medicinal materials
  • Method for detecting SUHs in traditional Chinese medicinal materials
  • Method for detecting SUHs in traditional Chinese medicinal materials

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0066] Experimental example 1 Methodology parameter research

[0067] Add a series of mixed standard solutions of concentrations to the blank sample, prepare a series of simulated samples of concentrations (marked samples), take the concentration as the abscissa C, and the peak area as the ordinate Y, and use the weighted least squares method to carry out linear regression analysis (weight The coefficient is 1 / C 2 ) to obtain a standard curve, the 7 kinds of SUHs have a good linear relationship within the range of 0.1-50ng / g, and the correlation coefficient r 2 Greater than 0.9913. The limit of detection (LOD) was 0.01-0.5ng / g and the limit of quantification (LOQ) was 0.1-2.0ng / g calculated by 3-fold and 10-fold signal-to-noise ratio. Prepare simulated samples with mass concentrations (2.0, 10, and 40ng / g), analyze 5 samples for each concentration, measure continuously for 3 days, calculate the mass concentration of each sample according to the standard curve of the day, and...

experiment example 2

[0072] Experimental Example 2 Extraction Efficiency Research

[0073] Add 50ng / g SUHs standard solution to the blank sample respectively to obtain the sample to be tested. The QuEChERS method and the method for detecting SUHs in Chinese medicinal materials provided by the present invention are respectively used for pretreatment of the samples to be detected, and the HPLC-MS / MS method is used to measure the SUHs content. Liquid mass conditions: the chromatographic column is a Water XBridge C18 column (100mm×4.6mmI.D., 3.5μm); the mobile phase is acetonitrile-0.1% formic acid aqueous solution (60:40, v / v) for isocratic elution, and the flow rate is 1.0 mL·min-1, the column temperature is 30°C, the ESI ion source is detected in positive ion mode, the spray voltage is 4000V, and the capillary temperature is 370°C.

[0074] Test results such as Figure 5 As shown, it can be seen that the method for detecting SUHs in Chinese herbal medicines provided by the present invention has h...

experiment example 3

[0075] Experimental example 3 Comparison of detection results of different Chinese herbal medicines

[0076] (1) Astragalus

[0077]Take 1g of astragalus powder, soak in 2mL of water and 5mL of acetonitrile, adjust the pH of the solution to 7, add 1.5g of MgSO 4 After dehydration with 0.35g NaCl, add 50mg of PSA, C18 and GCB material purification solution, after centrifugation, add 10mg of ZnAl-LDH material to the supernatant solution, vortex dispersion for 5min, after centrifugation, add a volume concentration of 5% trifluoro 200 μL of acetic acid solution was used to dissolve the solid-phase extraction product, and the content of SUHs was determined by HPLC-MS / MS.

[0078] Liquid mass conditions: the chromatographic column is a Water XBridge C18 column (100mm×4.6mm I.D., 3.5μm); the mobile phase is acetonitrile-0.1% formic acid aqueous solution (60:40, v / v) for isocratic elution, and the flow rate is 1.0mL. min-1, the column temperature is 30°C, the ESI ion source is detec...

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Abstract

The invention provides a method for detecting SUHs in traditional Chinese medicinal materials, and belongs to the technical field of food detection. The method comprises the following steps: adding a solid-phase extraction material into a first extraction solution obtained by adopting a QuEChERS method, enriching SUHs contained in the first extraction solution, and directly dissolving layered double hydroxides enriched with SUHs in an acidic solution to prepare a solution to be detected; according to the method, the concentration of the SUHs in the to-be-detected liquid is effectively improved, the influence of background substances in the first extraction liquid is further reduced, and the detection sensitivity, the detection precision and the selectivity of the SUHs are improved. The method for detecting the SUHs in the traditional Chinese medicinal materials is combined with an HPLC-MS / MS (High Performance Liquid Chromatography-Mass Spectrometry / Mass Spectrometry) method to detect the SUHs in the traditional Chinese medicinal materials, so that the time consumption for detecting a single sample is relatively short, the detection efficiency is high, the detection sensitivity is relatively good, and the detection limit of part of SUHs is as low as 0.01 ng / g.

Description

technical field [0001] The invention belongs to the technical field of food detection, in particular to a method for detecting SUHs in Chinese medicinal materials. Background technique [0002] Chinese herbal medicines will inevitably be attacked by various diseases and insect pests during the growth process, and it is inevitable to use pesticides. Unreasonable spraying of pesticides will inevitably lead to excessive pesticide residues in Chinese herbal medicines, and through the accumulation of food chains, it will cause serious damage to human health. At the same time, the problem of pesticide residues in Chinese medicinal materials has also become a bottleneck in my country's foreign export trade, seriously restricting the influence of Chinese medicine in the international market. [0003] Sulfonylurea herbicides (SUHs) have become one of the mainstream herbicides in the world due to their high efficiency, low dosage, and high selectivity. They are widely used in the contr...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/34
CPCG01N30/02G01N30/06G01N30/34
Inventor 邸欣任廷泽郭晓丽
Owner NINGXIA MEDICAL UNIV
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