Method for detecting 11 organophosphorus pesticide residues in radix paeoniae alba by ultra-high performance liquid chromatography-mass spectrometry

An organophosphorus pesticide and ultra-high performance liquid phase technology, which is applied in the field of chemical analysis and detection, can solve the problems of prone to false positive results, long growth cycle of white peony root, limited application range, etc., and achieve low detection limit and high accuracy High, high-sensitivity effects

Active Publication Date: 2019-12-24
NINGBO LIWAH PHARM CO LTD +3
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Radix Paeoniae Alba is susceptible to various diseases and insect pests in the planting process and has a high incidence rate. The abuse of pesticides has caused direct pollution of Radix Paeoniae Alba. In addition, the growth cycle of Radix Paeoniae Alba is long (generally 3-4 years), and the residual pesticides in the soil and air are easy to Accumulation in plant tissue will cause indirect pollution to Paeoniae Alba
[0003] At present, gas chromatography or gas-mass spectrometry are mostly used for the detection of organophosphorus pesticides. Gas chromatography is generally combined with a nitrogen-phosphorus detector (NPD) or a flame photometric detector (FPD), and both NPD and FPD are dedicated detectors. limited, and prone to false positive results; Wang Jiafeng et al. determined 10 organophosphorus pesticide residues in Radix Paeoniae Alba by gas-phase tandem mass spectrometry. Gel permeation chromatography was used for purification, which was costly and complicated to operate; Liu Xiaoqin et al. determined 99 kinds of pesticide residues in Radix Paeoniae Alba by gas chromatography-triple quadrupole tandem mass spectrometry. This method can realize the simultaneous determination of 99 kinds of pesticide residues, but some The repeatability RSD of pesticides is greater than 15%, and the reproducibility is poor, so it is necessary to explore a rapid sample processing and accurate quantitative detection method

Method used

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  • Method for detecting 11 organophosphorus pesticide residues in radix paeoniae alba by ultra-high performance liquid chromatography-mass spectrometry
  • Method for detecting 11 organophosphorus pesticide residues in radix paeoniae alba by ultra-high performance liquid chromatography-mass spectrometry
  • Method for detecting 11 organophosphorus pesticide residues in radix paeoniae alba by ultra-high performance liquid chromatography-mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Embodiment 1: the investigation of specificity

[0075] Preparation of 11 kinds of organophosphorus pesticide stock solutions: Weigh 10 mg of each of the 11 kinds of organophosphorus pesticide standard substances and place them in a 10mL volumetric flask, dissolve them with acetone and set the volume to the mark, so that the concentrations of the 11 kinds of pesticide standard substance stock solutions are 1000μg / mL, the pesticide standard stock solution is stored at -18°C;

[0076] Preparation of 1 μg / mL mixed reference solution: take 100 μL of each of the above 1000 μg / mL, and dilute to 10 mL with acetone to obtain a 10 μg / mL mixed standard solution; take 1 mL of 10 μg / mL mixed standard solution, add acetonitrile to dilute to 10mL to obtain a 1μg / mL mixed standard solution, see Attached Table 1 for details;

[0077] Preparation of 400ng / mL mixed reference substance solution: Take 400μL of the above 1μg / mL mixed reference substance solution, add acetonitrile to dissol...

Embodiment 2

[0089] Embodiment 2: the investigation of injection volume

[0090] Preparation of 11 kinds of organophosphorus pesticide stock solutions: Weigh 10 mg of each of the 11 kinds of organophosphorus pesticide standard substances and place them in a 10mL volumetric flask, dissolve them with acetone and set the volume to the mark, so that the concentrations of the 11 kinds of pesticide standard substance stock solutions are 1000μg / mL, the pesticide standard stock solution is stored at -18°C;

[0091] Preparation of 1 μg / mL mixed standard solution: take 100 μL of each of the above 1000 μg / mL, dilute to 10 mL with acetone to obtain a 10 μg / mL mixed standard solution; take 1 mL of 10 μg / mL mixed standard solution, add acetonitrile to dilute to 10mL to obtain a 1μg / mL mixed standard solution, see Attached Table 1 for details;

[0092] Preparation of 50ng / mL mixed standard solution: take 50μL of the above 1μg / mL, add acetonitrile to 1mL, and obtain 50ng / mL mixed standard solution;

[0...

Embodiment 3

[0097] Embodiment 3: the investigation of purifying filler

[0098] Preparation of 11 kinds of organophosphorus pesticide stock solutions: Weigh 10 mg of each of the 11 kinds of organophosphorus pesticide standard substances and place them in a 10mL volumetric flask, dissolve them with acetone and set the volume to the mark, so that the concentrations of the 11 kinds of pesticide standard substance stock solutions are 1000μg / mL, the pesticide standard stock solution is stored at -18°C;

[0099] Preparation of 1 μg / mL mixed standard solution: take 100 μL of each of the above 1000 μg / mL, dilute to 10 mL with acetone to obtain a 10 μg / mL mixed standard solution; take 1 mL of 10 μg / mL mixed standard solution, add acetonitrile to dilute to 10mL to obtain a 1μg / mL mixed standard solution, see Attached Table 1 for details;

[0100] Chromatographic conditions: Chromatographic column: Proshell HPH-C18 2.7μm 3x100mm; mobile phase: acetonitrile-0.1% formic acid (containing 10mmol / L ammo...

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Abstract

The invention discloses a method for simultaneously detecting 11 organophosphorus pesticide residues in radix paeoniae alba by ultra-high performance liquid chromatography-mass spectrometry, and the method comprises the following steps of extracting a medicinal material of radix paeoniae alba by acetone ultrasonic, placing the extracting solution in a centrifuge tube carried with 90mg of graphitized carbon black for vortex purification, taking the supernatant liquid nitrogen to dry, adding acetonitrile to make up the volume, using ultra-high performance liquid chromatography-mass spectrometryto detect in multiple reaction monitoring modes, and carrying out quantification by a external standard matrix curve method. The 11 organophosphorus pesticides have a high linear fit in the range of 2.5-200ng / mL, the recovery rate of the 11 pesticides at a concentration of 0.05mg / kg is 70%-130%, the relative standard deviation is less than or equal to 15%, and the method detection limit is less than or equal to 0.002mg / kg. The method is fast, simple, high in sensitivity, high in precision and high in accuracy, and is suitable for the analysis and detection of 11 organophosphorus pesticides inradix paeoniae alba.

Description

technical field [0001] The invention relates to a method for detecting 11 kinds of organophosphorus pesticide residues in Radix Paeoniae Alba by using ultra-high performance liquid chromatography-mass spectrometry technology, and belongs to the field of chemical analysis and detection. Background technique [0002] Radix Paeoniae Alba is the dried root of Paeonia lactiflora Pall. Excavated in summer and autumn, washed, removed the head and tail and fine roots, boiled in boiling water to remove the outer skin or peeled and then boiled, and dried in the sun. Radix Paeoniae Alba has the functions of nourishing blood and regulating menstruation, astringing yin and stopping sweating, softening liver and relieving pain, and calming liver-yang. For blood deficiency and chlorosis, irregular menstruation, spontaneous sweating, night sweats, hypochondriac pain, abdominal pain, cramped pain in limbs, headache and dizziness. Radix Paeoniae Alba is susceptible to various diseases and i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 沈君子殷红陈永建马长雨孙光财武晓剑钱勇谢天培
Owner NINGBO LIWAH PHARM CO LTD
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