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QuEChERS-UPLC-MS/MS method for analyzing pesticide residues in roxburgh rose

A technology for pesticide residues and prickly pears, which is applied in the fields of analytical chemistry and agricultural product safety, can solve the problems of not being able to better meet the needs of rapid detection of prickly pears and their products, the limited detection range, and the long detection period, and shorten the pretreatment time. , Simple cost, less waste effect

Pending Publication Date: 2022-02-25
GUIZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a fast, sensitive, accurate and simple, durable and low-cost analytical method for pesticide residues in Rosa roxburghii, which is used to solve the existing detection methods with cumbersome steps, limited detection range, long detection cycle, and cannot Better meet the needs of rapid detection of thorn pear and its products

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  • QuEChERS-UPLC-MS/MS method for analyzing pesticide residues in roxburgh rose
  • QuEChERS-UPLC-MS/MS method for analyzing pesticide residues in roxburgh rose
  • QuEChERS-UPLC-MS/MS method for analyzing pesticide residues in roxburgh rose

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Embodiment 1

[0040] Embodiments of the present invention provide a method for rapidly analyzing pesticide residues in Rosa roxburghii, said analysis method comprising the following steps:

[0041] After crushing the roxburghii sample to be analyzed, it is subjected to sample pretreatment to obtain the test solution.

[0042] After crushing the roxburghii sample without pesticide residues, pipette a certain amount of ultrapure water and add it in, perform sample pretreatment on it, filter the membrane, and obtain a matrix solution;

[0043] Add pure organic solvents to pesticide standard products and use pure organic solvents to prepare pesticide standard product mother liquor standard product solution mother liquor with a certain set concentration, pipette equal amounts of each pesticide standard product mother liquor into two volumetric flasks, and then use pure organic The solvent is fixed to volume to obtain the mixed intermediate solution of two solvent standards;

[0044] Use pure orga...

Embodiment 2

[0066] 1. Experimental part

[0067] 1.1 Instruments and reagents

[0068] Ultra-high performance liquid chromatography-tandem mass spectrometer (including Agilent 1290Infinity II ultra-high performance liquid chromatography and Agilent 6470 triple quadrupole mass spectrometer) (Agilent, USA); MS200 multi-tube vortex mixer (Hangzhou Ruicheng Instrument Co., Ltd. ); 1-16 small high-speed centrifuge (Sigma, Germany); CK2000 high-throughput tissue grinder (Beijing Tomorgen Biotechnology Co., Ltd.); BY-400B centrifuge (Beijing Baiyang Medical Instrument Co., Ltd.); AL104 analysis Balance (Mettler-Toledo).

[0069] C 18 (40-60μm), PSA (40-60μm), Tianjin Bona Agel Technology Co., Ltd.; Florisil (100-200 mesh), Sinopharm Chemical Reagent Co., Ltd.; GCB, Shanghai Aladdin Biochemical Technology Co., Ltd. Company; Anhydrous Magnesium Sulfate (Analytical Pure), Tianjin Yongda Chemical Reagent Co., Ltd.; Sodium Chloride (Analytical Pure), Methanol (Analytical Pure), Tianjin Kemiou Chem...

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Abstract

The invention discloses an economical, rapid, sensitive and accurate analysis method capable of simultaneously determining 11 common pesticide residues in roxburgh rose. The method comprises the following steps: crushing a sample, pre-treating by using an optimized QuEChERS method, taking acetonitrile as an extracting agent, taking N-propylethylenediamine and graphitized carbon black as a purifying agent, and analyzing by combining an ultra-high performance liquid chromatography-tandem mass spectrometer; using an Agilent Eclipse Plus C18 column for separation, 0.1% formic acid water-acetonitrile serving as a mobile phase, carrying out gradient elution, using an electrospray positive ion multi-reaction monitoring mode for detection, and using an external standard method for quantification. The method verifies that the method detection limit of 11 kinds of pesticides is between 1.31 mug / kg and 8.56 mug / kg, the quantification limit is between 4.13 mug / kg and 43.57 mug / kg, and the linear correlation coefficient (R) is between 0.9912 and 0.9999. According to the method, three concentration levels are selected for adding recovery rate experiments, the average adding standard recovery rate is 84.54%-103.81%, and the relative standard deviation (n=6) is 1.15%-8.46%. The method is rapid, sensitive and accurate in pretreatment, and can provide technical support for supervision of pesticides in rosa roxburghii tratt.

Description

technical field [0001] The invention relates to the technical fields of analytical chemistry and agricultural product safety, and mainly relates to a technique for measuring various pesticide residues in Rosa roxburghii, in particular to a QuEChERS-UPLC-MS / MS method for analyzing pesticide residues in Rosa roxburghii. Background technique [0002] Rosa roxburghii Tratt (Rosa roxburghii Tratt) scientific name reeling flower, belongs to Rosaceae Rosa plant, also known as mountain king fruit, thorn berry, frangipani, Ci pear, wood pear, alias thorn pineapple, send spring return, thorn pear, Prickly pear rose, nine-headed bird, wenxian fruit, and prickly pomegranate (Shaanxi) are rare nutritious and healthy fruits. Mainly Guizhou, Sichuan, Yunnan, Hubei, and Hunan have large distribution areas and high yields. Among them, Guizhou Province has the most wild prickly pears, which is also a unique advantageous resource in this province. Rosa roxburghii fruit is rich in multivitamin...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 吴小毛姚小龙安华明吴琼陈立杰韩磊罗跃刘旭东蔡武董艺博
Owner GUIZHOU UNIV
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