Detection method for residual quantity of cyanamide in fruits

A detection method, cyanamide technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as blank detection methods, no regulations on the maximum residue limit of cyanamide, incomplete dietary intake and risk data, etc.

Inactive Publication Date: 2017-12-12
SHANDONG YANTAI AGRI SCI & TECH INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the blank of the standard detection method of cyanamide residue in the field of cyanamide in the prior art, the dietary intake of cyanamide and the risk data of residents are incomplete, and the maximum residue limit value of cyanamide on food Provides a fast, simple and accurate method for the detection of cyanamide residues in agricultural products.

Method used

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  • Detection method for residual quantity of cyanamide in fruits
  • Detection method for residual quantity of cyanamide in fruits
  • Detection method for residual quantity of cyanamide in fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Main equipment and materials

[0032] Shimadzu LC / MS 8040; Guohua SHA-B constant temperature oscillator; Shanghai Yarong RE-52AA rotary evaporator (with Beijing Boyikang HX-1050 constant temperature circulator); fast mixer.

[0033] Methanol, acetone, ammonium acetate and formic acid were all chromatographically pure.

[0034] 2. Measurement method

[0035] (1). Standard curve drawing

[0036] Weigh the cyanamide solid and dilute it with acetonitrile to obtain 10 mg / kg and 1.0 mg / kg cyanamide solutions, pipette gun to draw 20 μL and 100 μL of 1.0 mg / kg cyanamide solutions into 2 stoppered test tubes respectively, Pipette 20 μL, 100 μL and 200 μL of 10 mg / kg cyanamide solution into three stoppered test tubes, add 0.5 mL of water, 0.05 g of sodium bicarbonate and 0.5 mL of 0.5% dansyl chloride acetone solution to each test tube .

[0037] Water bath and shake reaction at 50°C for 50-60min, then cool to room temperature, and dilute to 2 mL to obtain 0.01mg / kg, 0.05m...

Embodiment 2

[0054] 1. Main instruments and equipment (same as Example 1)

[0055] 2. Measurement method

[0056] (1) Standard curve drawing (same as Example 1)

[0057] (2) Sample extraction

[0058] Weigh 1.0g of grape samples homogenized by a wall breaker, add 10ml of ethyl acetate, vortex for 1min, then add 7g of anhydrous sodium sulfate, continue vortexing for 1min, filter with filter paper, rinse twice with 10ml of ethyl acetate , the filtrate was evaporated under reduced pressure in a rotary evaporator at 30°C to nearly dryness, and the volume was adjusted to 1 mL with acetone to obtain the concentrated solution to be derivatized;

[0059] (3). Concentrate derivatization

[0060] Take 0.5mL of the concentrated solution to be derivatized, add 0.5mL of water, 0.05g of sodium bicarbonate and 0.5mL of 0.5% dansyl chloride acetone solution, and shake it in a water bath at 50°C for 60 minutes to obtain a derivatized solution, which is connected to a liquid chromatography series The ma...

Embodiment 3

[0069] 1. Main instruments and equipment (same as Example 1)

[0070] 2. Measurement method

[0071] (1) Standard curve drawing (same as Example 1)

[0072] (2) Sample extraction

[0073] Weigh 5.0g of pear samples homogenized by a wall breaker, add 50ml of ethyl acetate, vortex for 1min, then add 35g of anhydrous sodium sulfate, continue vortexing for 1min, filter with filter paper, rinse twice with 10ml of ethyl acetate , the filtrate was condensed to the size of soybean grains through a rotary evaporator at 30°C in a water bath under reduced pressure, and added acetone to make the volume to 1 mL to obtain a concentrated solution to be derivatized;

[0074] (3). Concentrate derivatization

[0075] Take 0.5mL of the concentrated solution, add 0.5mL of water, 0.05g of sodium bicarbonate and 0.5mL of 0.5% dansyl chloride acetone solution, and shake it in a water bath at 50°C for 50-60min to obtain a derivative solution, and put it on a liquid chromatography series The mass ...

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Abstract

The invention relates to a detection method for the residual quantity of cyanamide in fruits. The detection method comprises the following specific steps: (1) standard curve drawing; (2) sample extraction; (3) concentrated solution derivation; (4) recovery rate measurement; (5) sample cyanamide content measurement. According to the detection method for the residual quantity of cyanamide in fruits, anhydrous sodium sulfate is used for removing water, ethyl acetate is extracted, after an extracting solution is concentrated, purification is avoided, the cyanamide can be directly derived with dansyl chloride, and the test operation is simple and convenient. By adopting a liquid chromatography tandem mass spectrometry multi-reaction monitoring mode, the detection method has relatively high selectivity and sensitivity, the interference of impurities can be effectively reduced, the detection method has relatively high accuracy and precision, and maximum residue limit is decided and technical support is provided for completing and supplementing cyanamide dietary intake and risk data of residents in next step.

Description

technical field [0001] The invention relates to the technical field of trace analysis, in particular to a method for detecting residual cyanamide in fruits. Background technique [0002] Cyanamide is not only a plant growth regulator, but also can be used as an insecticide and fertilizer, and is widely used in agriculture. However, there is currently no standard detection method for cyanamide residues in China, and the national standard GB 2763-2016 food safety national standard only stipulates the temporary limit of cyanamide on grapes. The main reason is that cyanamide has a small molecular weight, is easily soluble in water and is volatile, and it is difficult to extract and concentrate with common solvents. In addition, cyanamide has no chromophoric group, and is unstable when exposed to heat, acid, and alkali. It is very difficult to directly detect the residual amount of cyanamide without derivatization. In order to understand and understand the dietary intake leve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/12
CPCG01N30/02G01N30/12
Inventor 兰丰刘传德王志新姜蔚
Owner SHANDONG YANTAI AGRI SCI & TECH INST
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