Pre-treating extraction method for detecting melamine in soil and fertilizer
A technology for melamine and an extraction method is applied in the extraction field for pretreatment for determination of melamine in soil and fertilizers, and can solve the problems of less research on melamine extraction methods and poor extraction effect, etc.
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Embodiment 1
[0015] Example 1 The extraction effect of mechanical vibration is obviously better than that of ultrasonic vibration
[0016] 1) Ultrasonic extraction step: Weigh 1 g of four fertilizer samples (accurate to 0.1 mg) into a 50 mL centrifuge tube, add 25 mL of ammonia methanol solution, ultrasonicate for 30 min, centrifuge for 5 min, and pour the supernatant into another 50 mL centrifuge tube; Add 25mL ammonia water methanol solution again, sonicate for 30min, centrifuge for 5min, mix the two supernatants, take 10mL extract and blow dry with nitrogen, dilute to 5mL with diluent, pass through 0.45μm organic filter membrane, and detect by HPLC.
[0017] 2) Mechanical vibration extraction step: Weigh 1g of fertilizer sample into a 100mL Erlenmeyer flask, add 30mL ammonia water methanol solution, shake for 30min, centrifuge for 5min, pour the supernatant into a 50mL centrifuge tube; add 30mL ammonia water methanol solution again, shake 30min, centrifuge for 5min, mix the two supernat...
Embodiment 2
[0022] Example 2 The basic organic compound is obviously better than other water-soluble organic compounds as the extraction solution
[0023] In order to select a better extract, we took a certain amount of fertilizer samples and did the following experiments:
[0024] 1) Weigh 1g of chemical fertilizer sample, shake with 30mL 5 / 85 / 10 ammonia water / methanol / water, 30mL 50 / 50 methanol / water, 30mL water, and 30mL mobile phase (such as: 15% acetonitrile salt buffer) respectively, shake for 30min, Extract twice, take 10mL of nitrogen blowing, dilute to 5mL, pass through 0.45μm organic filter membrane;
[0025] 2) Weigh 1g of fertilizer sample, add 1mL 5ppm melamine standard solution, respectively use 30mL 5 / 85 / 10 ammonia water / methanol / water, 30mL 50 / 50 methanol / water, shake for 30min, extract twice, take 10mL nitrogen blowing, set Make up to 5mL, pass through 0.45μm organic filter membrane;
[0026] 3) Weigh 1g of fertilizer sample, add 1mL of 500ppm melamine standard solution...
Embodiment 3
[0040] Example 3 The effect of using a buffered organic solvent containing a small amount of salt as a diluent is obviously better than that of a single organic solvent.
[0041] In order to determine the composition of the diluent, we conducted the following experiments:
[0042] After the fertilizer samples were extracted according to the aforementioned optimal extraction method, 10 mL was taken, blown dry with nitrogen gas, and fixed to volume with 5 mL of 20% methanol aqueous solution and 5 mL of 15% acetonitrile buffer solution respectively. See the attachment for HPLC test results figure 1 .
[0043] Through the comparison of the melamine standard spectrum and the assignment of the peaks, we can clearly see that the detection sensitivity is greatly improved when using 15% acetonitrile buffer as the constant volume solution.
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