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Method for determining prochloraz or metabolite of prochloraz in plant-derived food

A plant-derived, metabolite technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of complex steps, inability to detect, low sensitivity, etc., and achieve high sensitivity, convenient measurement, and good selectivity.

Inactive Publication Date: 2015-03-04
INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance liquid chromatography (HPLC) can only detect the residual amount of prochloraz, but cannot detect the residual amount of its metabolite 2,4,6-trichlorophenol, and its sensitivity is lower than that of gas chromatography. For example, Yuan Xiaoya et al. (Determination of prochloraz 2,4,6-trichlorophenol residues in bananas by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Yuan Xiaoya, Pan Yonggui, Wang Meiling, Dai Hua. Physical and Chemical Testing-Chemical Volume, 2014 No. 50 Volume) Determination of banana samples by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry, only the residual amount of prochloraz was detected, but 2,4,6-trichlorophenol was not detected
Zhang Shirui et al. (Determination of prochloramine residues in two tropical fruits by GC. Zhang Shirui, Yuan Hongqiu, Yin Guihao. Modern Pesticides, August 2010, Volume 9, Issue 4) used GC to detect prochloramine in fruits residues, 2,4,6-trichlorophenol was not detected at the same time, and its sample pretreatment steps were complicated

Method used

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  • Method for determining prochloraz or metabolite of prochloraz in plant-derived food
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  • Method for determining prochloraz or metabolite of prochloraz in plant-derived food

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Embodiment 1

[0070] Example 1 GC-MS / MS of the present invention detects prochloraz or its metabolite residues

[0071] 1. Preparation of standard stock solution

[0072] Accurately weigh 10 mg (accurate to 0.01 mg) of prochloraz, 2,4,6-trichlorophenol and N-propyl-2-(2,4,6-trichlorophenoxy) ethylamine standard substance respectively in In a 100mL volumetric flask, dissolve with acetonitrile and dilute to the mark, and prepare prochloraz standard stock solution, 2,4,6-trichlorophenol standard stock solution and N-propyl-2 -(2,4,6-Trichlorophenoxy)ethylamine standard stock solution, stored in -18°C refrigerator, for future use.

[0073] 2. Preparation of standard working solution

[0074] Accurately measure 1.0mL prochloraz standard stock solution, 2,4,6-trichlorophenol standard stock solution and N-propyl-2-(2,4,6-trichlorophenoxy)ethylamine standard stock solution respectively solution in a 50mL volumetric flask, dilute to the mark with acetonitrile, and prepare prochloraz standard work...

Embodiment 2

[0087] Example 2 GC-MS of the present invention detects prochloraz or its metabolite residues

[0088] The present invention also uses gas chromatography-mass spectrometry (GC-MS) to detect prochloraz or its metabolites in plant-derived foods, and the specific content is as follows:

[0089] Instruments and reagents

[0090] Gas chromatography spectrometer (Thermo Trace 1310ISQ); SIGMA 2-16K desktop centrifuge (Sartoriussigma, Germany); EYELA MMV-1000W oscillator (Tokyo, Japan); IKA vortex mixer; TruboVapII automatic concentrator.

[0091] Acetonitrile (chromatographically pure); PSA (N-propyl ethylenediamine), C18 (octadecylsilane bonded silica gel) (Tianjin Bona Agel Technology Co., Ltd.); anhydrous sodium sulfate, sodium chloride (analytical Pure, Guangzhou Chemical Reagent Factory), burned in a muffle furnace at 650°C for 4h before use; water was deionized water; standard prochloraz (DR, purity 99.0%), N-propyl-2-( 2,4,6-trichlorophenoxy)ethylamine standard was synthesiz...

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Abstract

The invention provides a method for determining prochloraz or metabolite of prochloraz in plant-derived food. The method comprises the following steps: a, selecting the plant-derived food, adding organic solvent and sodium chloride into the plant-derived food, uniformly mixing, centrifuging the mixture, standing for layering the mixture, and taking the supernatant; b, adding anhydrous sodium sulfate into the supernatant acquired in the step a, uniformly mixing the anhydrous sodium sulfate with the supernatant, standing the mixture, and taking the supernatant; c, concentrating the supernatant acquired in the step b, making the volume constant, adding anhydrous sodium sulfate, N-propylethylenediamine and octadecyl silane bonded silica gel into the supernatant, uniformly mixing the mass, centrifuging the mixture, and taking the supernatant as a sample to be detected; and d, detecting the sample by adopting GC-MS / MS or GC-MS (Gas Chromatography-Mass Spectrometer). According to the method, a specific detection condition is adopted, linear response is good, and the residue of prochloraz or metabolite of the prochloraz can be accurately, rapidly and conveniently determined; meanwhile, the method has advantages of simplicity, rapidness, good selectivity, high sensitivity and good matrix interference resistance.

Description

technical field [0001] The invention relates to a method for determining prochloraz or its metabolites in plant-derived foods. Background technique [0002] Prochloraz is a broad-spectrum imidazole fungicide, which can prevent and control powdery mildew, anthracnose and other diseases. Preservation and preservation during post-storage and transportation, and prevention and treatment of diseases during storage. The final metabolite of prochloraz is 2,4,6-trichlorophenol, which has high toxicity and poor biodegradability, which is likely to cause serious environmental pollution and is suspected to be a strong carcinogen. The United Nations Food and Agriculture Organization / World Health Organization (FAO / WHO) Codex Alimentarius Commission (CCPR) stipulates that the maximum residue limit of prochloraz on crops includes the sum of the residues of prochloraz and its metabolites. Therefore, it is necessary to detect and control the residues of prochloraz and its metabolites in fr...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 李蓉卢俊文杨芳张朋杰储大可黄思允陈丽斯
Owner INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY EXIT INSPECTION AND QUARANTINE
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