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Method for detecting residue quantity of depressant medicine in aquatic products

A sedative and residual technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of not high-resolution mass spectrometry, sedatives that have not been used, and the variety is not wide enough to achieve simple operation methods, good accuracy, and precision high effect

Active Publication Date: 2018-03-27
中山海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ultra-high performance liquid chromatography-quadrupole / electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) with high sensitivity, high selectivity and high mass precision has been used in pesticide residues, hypoglycemic Determination of drugs, polypeptide drugs, mycotoxins, etc. It has not been used to analyze sedatives in aquatic samples
Application number 201410197253.2 discloses a method for determining the residual sedative veterinary drugs in mutton. Although the method is described as high-resolution liquid chromatography-tandem mass spectrometry, it uses liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MSMS ) is not really high-resolution mass spectrometry, the method is suitable for the simultaneous detection of 15 sedative drugs, the category is not wide enough

Method used

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  • Method for detecting residue quantity of depressant medicine in aquatic products
  • Method for detecting residue quantity of depressant medicine in aquatic products
  • Method for detecting residue quantity of depressant medicine in aquatic products

Examples

Experimental program
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Effect test

Embodiment 1

[0036] A method for detecting the residual amount of sedative drugs in aquatic products, the sedative drugs are estazolam, midazolam, triazolam, alprazolam, nitrazepam, clonazepam, flunitrate Zepam, Oxazepam, Norazepam, Diazepam, Diazepam, Lorazepam, Propionyldimethazine, Azaperone, Acepromazine, Chlorpromazine, Azapine alcohol, promethazine, carbazolol, xylazine, fluphenazine, haloperidol, perphenazine, droperidol; the detection method includes the following steps:

[0037] (1) Sample pretreatment: take 1.50-2.50 g of the homogenized sample and place it in a 50 mL polypropylene centrifuge tube, add 4 g of sodium chloride, vortex for 30-40 seconds to mix, add 10 mL of acetonitrile, homogenize for 1-3 minutes, Sonicate for 10-15min; centrifuge at 4000-4500r / min for 5-10min, transfer the supernatant to another 50mL polypropylene centrifuge tube; add 10mL acetonitrile to the residue, shake for 5-10min, and centrifuge for 5-10min , combine the secondary supernatants, vortex and m...

Embodiment 2

[0045] Embodiment 2 Comparison of different liquid chromatography conditions

[0046] Comparing the separation effect of the chromatographic column Waters ACQUITY UPLC BEH C18 (2.1mm×100mm, 1.7μm) and Thermofisher Accucore RP-MS (100mm×2.1mm, 2.6μm), it was found that the Waters ACQUITYUPLC BEH C18 chromatographic column has a Higher column efficiency and better separation effect. Acetonitrile solution containing 0.1% (v / v) formic acid was selected as mobile phase A, and aqueous solution containing 0.1% (v / v) formic acid was selected as mobile phase B, and a gradient elution procedure was adopted. figure 1 It is the extracted ion current chromatogram of 24 sedatives with a concentration of 10 ng / mL in the blank grass carp matrix solution.

Embodiment 3

[0047] Example 3 Determination of mass spectrometry conditions

[0048] Using full scan of primary mass spectrometry plus data-dependent secondary mass spectrometry (Full MS / dd-MS2) (TopN=1), perform full scan of primary mass spectrometry for the selected mass number range (m / z100~1000) to find parent When the intensity of ions reaches the set threshold (1e6), the MS / MS scan is automatically triggered. While obtaining the accurate mass number of the parent ion, the full scan information of the secondary mass spectrum was also obtained. The compound was fragmented with three different normalized collision energies (Stepped(N)CE) of 20%, 40%, and 60%, and an adduct map with rich fragment ion information was obtained. Further adjust dynamic exclusion (Dynamicexclusion), apex trigger (Apex trigger), TopN and other parameters to obtain better fragment ion information. Dynamic exclusion compared 6s, 8s, and 10s, and the peak shape at 6s was better. Satisfactory secondary fragment...

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Abstract

The invention discloses a method for detecting the residue quantity of depressant medicine in aquatic products. The method can be used for detecting the medicine residue of 24 depressant medicines, and comprises the following steps of performing sample pretreatment; after sample homogenizing, adding salting-out agents; using acetonitrile for extraction; after concentration, using 50-percent (v / v)methanol-water solution for reaching the constant volume; then, using acetonitrile saturated n-hexane for purification; performing ultra-high performance liquid chromatography-quadrupole / static fieldorbitrap high-resolution mass spectrometric detection, wherein the chromatographic column uses ACQUITY UPLC BEHC18; using gradient elution; preparing mixed depressant medicine standard work solutionsof different concentrations; respectively performing mass spectrometric detection to obtain each depressant linear equation and corresponding decision coefficients; substituting the chromatographic peak area of the sample into the depressant medicine standard work solution equation to obtain the detection result. The method has the advantages that the operation is simple; the precision is high; the accuracy is high; in addition, the applicable depressant types are more.

Description

technical field [0001] The invention relates to a method for detecting residual drugs in aquatic products, in particular to a method for simultaneously detecting the residual amounts of multiple sedative drugs in aquatic products. Background technique [0002] Sedatives are also called movement inhibitors, because they can prevent animal commotion, trauma, mutual pecking and biting under high-density feeding or long-distance transportation, group transfer, high temperature and other stressful situations, and reduce production performance decline and product failure caused by various stresses. If the quality declines, it will be used illegally by humans, resulting in sedatives remaining in animal tissues, causing food safety problems. After a normal person ingests this kind of food, the burden on the liver will increase, the mind will be dizzy for a long time, the memory will be affected, and the motor nerve and muscle function will be inhibited. Announcement (No. 235) of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N30/72G01N2030/146
Inventor 李蓉杨璐齐刘恭源罗阳丹
Owner 中山海关技术中心
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