Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum

An ultra-high performance liquid phase, series quadrupole technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to analyze and detect multiple types of pesticide residues at the same time, cumbersome analysis process, long analysis time, etc., and achieve a linear relationship. Good, selective, low pollution effect

Active Publication Date: 2012-10-17
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, there are problems such as long analysis time, inability to analyze and detect multiple types of pesticide residues at the same time, cumbersome analysis process, and high cost.

Method used

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  • Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum
  • Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum
  • Method for simultaneously determining one hundred pesticide residuals in traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum

Examples

Experimental program
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Effect test

preparation example Construction

[0045] [1] Preparation of pesticide standard stock solution: Weigh 10 mg each of 100 kinds of pesticide standards and put them in 10mL volumetric flasks, choose acetonitrile, methanol or acetone to dissolve the pesticide standards respectively and set the volume to the mark, so that 100 kinds of pesticide standards The concentrations of the stock solutions of pesticides were all 1000 μg / mL, and the stock solutions of pesticide standards were stored at -18°C.

[0046] [2] Preparation of pesticide mixed standard solution: Take out the above-mentioned 100 kinds of pesticide standard stock solutions respectively, then mix them together, dilute to volume with acetonitrile, and use each pesticide standard in Table 3 in the pesticide mixed standard solution Prepare the pesticide mixed standard solution.

[0047] [3] Preparation of ginseng pretreatment solution: ①Crush the ginseng decoction pieces to be tested, pass through a No. 9 sieve to obtain the ginseng sample powder to be teste...

Embodiment 2

[0068] [Example 2] Take Flos Lonicerae as a representative of flowering Chinese herbal medicines.

[0069] [1] Preparation of pesticide standard stock solution; [2] Preparation of pesticide mixed standard solution is the same as in Example 1;

[0070][3] Preparation of honeysuckle pretreatment solution: ①Crush the decoction pieces of honeysuckle to be tested, pass through a No. 9 sieve to obtain the ginseng sample powder to be tested, and store it in a desiccator; ②Take 2.00g of the honeysuckle sample powder to be tested, add 10mL of ultrapure water, mix well and let it stand for 1 hour, add 10mL of acetic acid-acetonitrile mixture with a volume fraction of 0.1% acetic acid and extract by vortex for 1min; ③add 4g of anhydrous magnesium sulfate and 1g of chlorine to the above extract Continue to vortex extract the sodium chloride mixture for 1 min; ④Centrifuge at 3500rpm for 10min at 4°C; The supernatant was blown dry with nitrogen, and was fixed to 1 mL with a mixed solution ...

Embodiment 3

[0091] [Example 3] Cornus officinalis is used as a representative of fruit Chinese medicinal materials.

[0092] [1] Preparation of pesticide standard stock solution; [2] Preparation of pesticide mixed standard solution is the same as in Example 1.

[0093] [3] Preparation of Cornus officinalis pretreatment solution: ①Crush the decoction pieces of Cornus officinalis to be tested, pass through a No. 9 sieve to obtain the ginseng sample powder to be tested, and store it in a desiccator; 10mL of ultrapure water, mix well and let it stand for 1 hour, add 10mL of acetic acid-acetonitrile mixture with a volume fraction of 0.1% acetic acid and extract by vortex for 1min; ③add 4g of anhydrous magnesium sulfate and 1g of chlorine to the above extract Continue to vortex extract the sodium chloride mixture for 1 min; ④Centrifuge at 3500rpm for 10min at 4°C; The supernatant was blown dry with nitrogen, and the mixed solution of methanol and water containing 0.1% formic acid was used to m...

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Abstract

The invention provides a method for simultaneously determining one hundred pesticide residuals in a traditional Chinese medicine through ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum. The method comprises the following steps: immersing traditional Chinese medicine powder with ultrapure water, extracting with acetonitrile containing 0.1% acetic acid through a homogenate method, carrying out solid phase dispersing purification with N-propylethylenediamine and graphitized carbon, detecting in a timesharing multi-reaction monitoring mode through the ultrahigh performance liquid chromatography-tandem quadrupole mass spectrum, and quantifying with an external standard curve method. 88% of pesticides have good linear relations in a range of 5-500ng/mL, correlation coefficients are above 0.99, and the correlation coefficients of above 98% of the pesticides are above 0.97; the average recovery rate of the pesticides with the low concentration of 10mug/kg, the middle concentration of 50mug/kg and the high concentration of 100mug/kg is 70-130%, and the relative standard deviation is less than 0.15; and the detection limit is equal to or less than 0.01mg/kg, so routine detection requirements can be completely satisfied. The method has the advantages of strong versatility, good selectivity, high sensitivity, and rapidness and simplicity.

Description

field of invention [0001] The invention belongs to the field of analytical chemistry. Specifically, the invention relates to an ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry method for simultaneously analyzing the contents of 100 kinds of pesticide residues in traditional Chinese medicines. technical background [0002] Pesticide residue refers to the general term of the pesticide original body, toxic metabolites, degradation products and impurities remaining in organisms, agricultural by-products and the environment after pesticide use. The invention and use of pesticides have brought many negative effects while increasing crop yields. [0003] As a special substance, traditional Chinese medicine has an increasing demand due to its unique effects in treating diseases and strengthening the body. At present, wild medicinal materials are far from meeting the market demand, and most Chinese herbal medicines rely on artificial cultivation. In ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 刘志强陈丽娜宋凤瑞郑重邢俊鹏刘淑莹
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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