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Method for determination of pesticide residues in vegetable oils

A technology for pesticide residues and vegetable oils, applied in the field of determination of pesticide residues in vegetable oils, can solve the problems of high detection limit, poor sensitivity, and powerlessness of qualitative identification

Inactive Publication Date: 2014-03-26
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, traditional detection methods mostly use gas chromatography (GC) and gas chromatography-mass spectrometry (GC / MS). The sensitivity of the method itself is relatively poor, resulting in a high detection limit of the method
However, these technologies with high-efficiency separation capabilities are powerless in the qualitative identification of the separated components.

Method used

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  • Method for determination of pesticide residues in vegetable oils
  • Method for determination of pesticide residues in vegetable oils
  • Method for determination of pesticide residues in vegetable oils

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1: Optimization of chromatographic conditions

[0053] The properties of the 104 target compounds to be detected are quite different, and the choice of the mobile phase system plays an important role in the separation effect. In this example, in acetonitrile-water, methanol-water, methanol-ammonium acetate solution, ammonium acetate methanol solution - Select the best mobile phase system among the four solutions of ammonium acetate aqueous solution.

[0054]The column conditions are as follows:

[0055] Restek C18 chromatographic column (3μm, 2.1×100mm, Restek, USA);

[0056] Column temperature: 35°C;

[0057] Balance time: 5min;

[0058] Injection volume: 10μL;

[0059] Flow rate: 0.5mL / min;

[0060] Mobile phase: use the mobile phase composed of solution A and solution B for gradient elution, elution conditions: 0-8min, B from 20.0%-90.0%; 8-12min, B from 90.0%-100.0%; 12-14.8min , B maintained at 100.0%; 14.8-14.9min, B from 100.0%-20.0%; 15.0min sto...

Embodiment 2

[0072] Embodiment 2: Optimization of extraction reagents in mass spectrometry conditions

[0073] In this example, the APCI source and the ESI (+) ion source were selected. The experiment found that the noise baseline of the APCI source is low, but the response value of the target is also low, and the response under the ESI (+) condition is better, which meets the sensitivity requirement. Using a peristaltic pump to continuously inject at a flow rate of 10 μL / min, respectively inject 0.5 mg / L pesticide standard solutions into the ESI ion source, perform primary mass spectrometry analysis (Q1 scan) in positive ion detection mode, and obtain quasi-molecular ion peaks [ M+H]+, optimized declustering voltage. Perform secondary mass spectrometry analysis (product ion scanning) on ​​quasi-molecular ion peaks to obtain full spectrum information of secondary mass spectrometry fragments, optimize collision energy, and establish a standard substance EPI spectral library at the same time...

Embodiment 3

[0086] Example 3: Optimization of Freezing Time in Mass Spectrometry Conditions

[0087] After optimizing the extraction steps, although most of the oil remained in the residue, a small part still entered the acetonitrile layer. In order to further purify, freezing was used to remove the oil. In the optimization of freezing time, 0h, 0.5h, 1.0h, 2.0h, 4.0h and 6.0h were selected as the optimization time selection scheme. Put the acetonitrile extraction layers obtained by different extraction methods into the -18°C refrigerator to freeze at the same time, take out 2mL of the extracts at intervals, dry them and weigh them, and use the subtraction method to draw the freezing effect curve, see image 3 . image 3 It is a freezing time optimization diagram, wherein, A, B, C, D, E, and F respectively represent the six extraction schemes of A-F in Example 2.

[0088] from image 3 It can be clearly seen that with the extension of freezing time, the oil content in the extract drops...

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Abstract

The invention discloses a method for determination of pesticide residues in vegetable oils, and the method includes (1) sample treatment; (2) preparation of a standard solution; (3) chromatographic conditions: a Restek C18 chromatographic column, column temperature of 35 DEG C, equilibrium time of 5min, injection volume of 10 muL, flow rate of 0.5mL / min, mobile phases comprising A 10mMol ammonium acetate aqueous solution and B 10mMol ammonium acetate methanol solution; (4) mass spectrometry conditions: an electrospray ion (ESI) source, positive ion scan, a programmed multiple reaction monitoring mode, curtain gas of 15L / min, GS1 atomization gas of 60L / min, GS2 auxiliary heating gas of 70L / min, a medium CAD (collision-activated dissociation) collision gas, auxiliary heating gas temperature of 500 DEG C and spray voltage of 5000v. The high throughput detection method for variety of pesticide residues in three commonly used vegetable oils comprising olive oil, palm oil and peanut oil is established and is used for quality control of the vegetable oils.

Description

technical field [0001] The invention relates to a method for determining pesticide residues in vegetable oil, in particular to a method for determining one or more pesticide residues in vegetable oil by combining dispersive solid-phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry. Background technique [0002] With the improvement of agricultural science and technology and economic level, agricultural products have basically met the requirements of quantity security, and people are paying more and more attention to the quality and safety of agricultural products and food. my country is the world's largest consumer of vegetable oil, but our research on pesticide residues in vegetable oil lags far behind the international level. [0003] The high oil content of vegetable oil makes the extraction and purification of pesticide residues very difficult. Therefore, it is the key to establish a multi-pesticide residue detection method to effec...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 徐娟王岚李荀陈捷
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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