Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer

A two-dimensional gas chromatography and time-of-flight mass spectrometry technology, applied in the field of food safety, can solve the problems of large reagent consumption, time-consuming, easy decomposition, etc., and achieve good extraction and purification effects, increase accuracy, and save reagents.

Inactive Publication Date: 2013-10-30
ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The pretreatment methods of pesticide residues in traditional Chinese medicine mainly include solvent extraction, accelerated solvent extraction, liquid-liquid distribution, and solid-phase microextraction. high cost issues

Method used

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  • Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer
  • Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer
  • Method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Instruments and reagents

[0055] Instrument: Leco Pegasus4D GC×GC—TOF—MS time-of-flight mass spectrometer (Leco, USA); equipped with Agilent7890 two-dimensional gas chromatograph, Gerstel MPS2 (Gerstel GmbH, Mülheim der Ruhr, Germany) autosampler, tissue homogenizer (Germany IKA company), rotary evaporator (Switzerland Buchi company), high-speed refrigerated centrifuge (Japan Hitachi CR G Series), centrifuge (Japan Sigma2-16PK), filter receiving device 47mm, 250mL (Thermo Fisher Scientific Corporation ) Inorganic aluminum oxide film 0.02μm, 47mm (Whatman company).

[0056] Acetonitrile, acetone, HPLC grade, purchased from Dima Company, 2mL purification tube including N-propylethylenediamine (PSA) adsorbent 50mg, anhydrous magnesium sulfate 150mg, purchased from Waters Company (DisQue Dispersive SPE Kit), Graphite carbon black (purchased from SEPAX-UCT, USA), sodium chloride, analytically pure. 103 kinds of pesticide standard products (purity not less than 95%, pur...

Embodiment 2

[0073] The sample of Schisandra chinensis was tested by gas chromatography electron capture detector (ECD), and cypermethrin was detected, and the sample was verified as an interfering substance by two-dimensional gas chromatography-time-of-flight mass spectrometry, and cypermethrin was not detected in the sample.

[0074] Instruments and reagents

[0075] Gas chromatographic conditions: Agilent 7890A, equipped with ECD detector, chromatographic column DB-35MS temperature rise program: 150°C for 1min, 10°C per minute to 280°C for 30min, injection port: 250°C, split injection, Split ratio 10:1 detector: 300°C

[0076] Petroleum ether and ethyl acetate are chromatographically pure, purchased from Dima Company, and the finished Fluori column is purchased from Chromatography Company

[0077] Pre-treatment method: Weigh 10g of the ground Schisandra chinensis sample into a 100mL Erlenmeyer flask, add 20mL of petroleum ether, shake on the oscillator for 30min, let it stand, and take 2...

Embodiment 3

[0085] The schisandra sample utilizes the method of the present invention to detect cypermethrin, triadimenol and metolachlor.

[0086] The instrument conditions and pretreatment method are the same as in Example 1. As a result, the Schisandra chinensis sample utilizes the method of the present invention to detect 0.06 mg / kg of cypermethrin, 0.02 mg / kg of triadimenol, and 0.01 mg / kg of metolachlor. The spectrogram is shown in Figure 7 , the mass spectrum of cypermethrin was detected in Figure 8

[0087] Add 103 pesticide standard mixed solutions at four levels of 0.01mg / kg, 0.05mg / kg, 0.1mg / kg, and 0.25mg / kg to 10 kinds of matrices such as ginkgo biloba, schisandra, and ginseng to complete the standard recovery experiment, and 90% The recovery rate of the pesticide method is between 60% and 120%, the relative standard deviation is less than 20%, and the detection limit of the method is 0.01 to 0.05mg / kg, which meets the limit requirements of pesticide residues in traditiona...

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Abstract

The invention discloses a method for quickly detecting pesticide multiple residues in traditional Chinese medicine through membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometer. The method comprises the following steps: extracting the pesticide residues of a traditional Chinese medicine sample through acetonitrile, carrying out ultrafiltration separation of an inorganic alumina oxide membrane, allowing the sample extraction solution to be subjected to solid-phase dispersing, extraction and purifying, and carrying out detection by the comprehensive two-dimensional gas chromatography--time-of-flight mass spectrometer, wherein the comprehensive two-dimensional gas chromatography adopts two chromatographic columns in different polarities to perform orthogonal separation to base material and to-be-detected components of the medicine base material, the base material and the to-be-detected components enter a time-of-flight mass spectrometer under the action of a modulator-demodulator for completing qualitative and quantitative detection, and an external standard method is adopted to complete quantization. The method provided by the invention has the characteristics of quickness, simplicity and convenience, high sensitivity, good separation effect, reagent conservation, accurate and reliable qualitativeness and quantization, and the like, and solves the problems that the complex base materials, such as the pesticide residues of the traditional Chinese medicine, are difficult to separate and in qualitativeness and quantization.

Description

technical field [0001] The invention belongs to the technical field of food safety, and relates to a method for rapidly detecting multiple residues of pesticides in traditional Chinese medicines by using membrane separation and comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry. Background technique [0002] my country is a big country in the cultivation, use and export of traditional Chinese medicine, and its medicinal efficacy has been increasingly recognized by consumers at home and abroad. In recent years, due to improper planting, environmental pollution or profit-driven, the problem of pesticide residue pollution in artificial planting of traditional Chinese medicine has continuously appeared, which has become an important factor affecting the efficacy and safety of drugs, and the harm to humans and the environment cannot be ignored. Concerns about pesticide residues in traditional Chinese medicine are on the rise. At present, Europe, Ame...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 王云凤高健会刘旸
Owner ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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