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.
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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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