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Hot pepper and determining method for 96 pesticide residues in product of hot pepper

A technology for pesticide residues and determination methods, which is applied in the field of pesticide residue determination and achieves the effects of good repeatability, high sensitivity and easy operation.

Active Publication Date: 2014-01-15
INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at present, there are no reports on the detection methods of 96 kinds of pesticide residues in peppers exported to Korea at home and abroad.

Method used

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  • Hot pepper and determining method for 96 pesticide residues in product of hot pepper
  • Hot pepper and determining method for 96 pesticide residues in product of hot pepper
  • Hot pepper and determining method for 96 pesticide residues in product of hot pepper

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: the detection of 96 kinds of pesticide residues in frozen pepper

[0046] (1) extract

[0047] Weigh 10.0 g of fully mixed frozen pepper into a 50 mL centrifuge tube, accurately add 25 mL of 1% acetic acid acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate, 2 g of sodium acetate and 5 mL of water, shake vigorously for 1 min, and centrifuge at 7000 r / min Wait for purification after 5min.

[0048] (2) Purification of 69 pesticide residues determined by GC-MS

[0049] Take 5 mL of the upper layer extract in a test tube, add 50 μL of n-decane, blow with nitrogen gas at 40 °C until nearly dry, add 2 mL of acetone / n-hexane (1 / 1, volume ratio, the same below) to dissolve the residue. Pre-wash the Florisil solid-phase extraction column with 5mL acetone / n-hexane, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetone / n-hexane, and transf...

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Abstract

The invention discloses hot pepper and a determining method for 96 pesticide residues in a product of the hot pepper. The determining method comprises the following steps: homogenously extracting residual pesticide in a sample with 1% acetic acid-acetonitrile solution, purifying the extracting solution with a Florisil solid phase extraction column, dispersing and purifying the extracting solution with ethylenediamine-N-propyl silane (PSA) and octadecyl silane bonded phase (C18) substrate, detecting 69 pesticide residuals in the purified concentrated liquid of the Florisil column by GC-MS (gaschromatographic mass spectrometry), detecting 27 pesticide residuals in the substrate dispersed purified liquid by liquid chromatography-tandem mass spectrometry (LC-MS / MS), using the black substrate solution dilution standard to construct the updated calibration curves, adopting an internal standard method to quantify when using GC / MS to detect the residuals, and adopting an external standard method to quantify when using LC-MS / MS to detect the residuals. The average recovery rate of the method is 70.7-118.6%; the average relative standard deviation (RSD) is 3.2-11.4%; the detection limit is 0.13-28.2 ug / kg. The determining method has the advantages of simplicity and convenience in operation, high speed, accuracy, high sensitivity and good repeatability.

Description

Technical field [0001] The invention relates to a method for measuring 96 kinds of pesticide residues in peppers and their products, and belongs to the technical field of measuring pesticide residues. Background technique [0002] Vegetables and fruits are an important part of a balanced human diet. The quality and safety of vegetables and fruits are very important. In recent years, due to incorrect and irrational use of pesticides, incidents of contaminating vegetables and fruits and causing pesticide poisoning have continued to occur. In order to ensure the safety of national consumers and protect the orderly conduct of international trade, many countries have formulated maximum residue limits (MRL) standards for pesticides in agricultural products to ensure food safety. At the same time, in international trade, MRL is also used by some countries and regions as a tool to build technical trade barriers. [0003] Chili peppers and their products are my country's important ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 崔淑华刘润珠刘靖靖汤志旭王建华王境堂
Owner INSPECTION & QUARANTINE TECH CENT SHANDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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