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A kind of extraction method used for pretreatment of melamine determination in soil and fertilizer

A technology for melamine and an extraction method, which is applied in the extraction field for pretreatment for the determination of melamine in soil and fertilizers, can solve the problems of poor extraction effect and less research on melamine extraction methods.

Inactive Publication Date: 2016-05-11
上海出入境检验检疫局工业品与原材料检测技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although the detection method of melamine is mature, there are few studies on the extraction method of melamine, and the extraction effect of melamine in soil and fertilizer reported in some existing literature is not good, so the extraction method of melamine in soil and fertilizer is optimized , in order to truly measure the content of melamine in the above samples, which is of great significance to the quality safety and supervision of melamine in fertilizers

Method used

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  • A kind of extraction method used for pretreatment of melamine determination in soil and fertilizer
  • A kind of extraction method used for pretreatment of melamine determination in soil and fertilizer
  • A kind of extraction method used for pretreatment of melamine determination in soil and fertilizer

Examples

Experimental program
Comparison scheme
Effect test

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 fertilizer sample, use 30mL5 / 85 / 10 ammonia water / methanol / water, 30mL50 / 50 methanol / water, 30mL water, 30mL mobile phase (such as: 15% acetonitrile salt buffer), shake for 30min, extract two For the second time, take 10mL nitrogen blowing, dilute to 5mL, and pass through a 0.45μm organic filter membrane;

[0025] 2) Weigh 1g of fertilizer sample, add 1mL of 5ppm melamine standard solution, respectively use 30mL of 5 / 85 / 10 ammonia / methanol / water, 30mL of 50 / 50 methanol / water, shake for 30min, extract twice, take 10mL of nitrogen blowing, and dilute to 5mL , through a 0.45μm organic filter membrane;

[0026] 3) Weigh 1g of fertilizer sample, add 1mL of 500ppm melamine standard solution, respectiv...

Embodiment 3

[0041] 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.

[0042] In order to determine the composition of the diluent, we conducted the following experiments:

[0043] After the fertilizer samples were extracted according to the aforementioned optimal extraction method, 10 mL was taken, blown dry with nitrogen, 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 .

[0044] by attaching figure 1 In the comparison of the standard chromatogram of melamine and the attribution of the peak, we can clearly see that when 15% acetonitrile buffer solution is used as the constant volume solution, the detection sensitivity is obviously higher than that of 20% methanol water. figure 1 The peak in spectrum 1 is higher than the peak in spectrum 2).

[0045] ...

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Abstract

The invention provides a method which is scientific and reasonable, strong in operability, and wide in applicability, and according to the method, results are satisfying by means of addition standard recovery and standard control. The invention relates to a pre-treating extraction method for detecting melamine in soil and a fertilizer. According to the method, the best extraction condition for detecting the melamine in the soil and the fertilizer can be obtained by optimizing a plurality of parameters such as an extraction way, the composition of an extracting solution and the composition of a diluted solution, so that the content of the melamine in the sample is detected precisely, factually and reliably. The pre-treating extraction method can be applied to the detection of the melamine in the same product. The method is scientific and reasonable, strong in operability, and wide in applicability, and according to the method, the results are satisfying by means of the addition standard recovery and the standard control.

Description

1. Technical field [0001] The present invention relates to an extraction method used for the pretreatment of the determination of melamine in soil and fertilizers. The method has great innovations in the extraction method, selection of extraction solution and dilution solution, etc., and can truly and effectively determine the melamine in the above soil and fertilizer samples. The content of melamine, its extraction effect is very satisfactory. 2. Background technology [0002] Melamine, which is added to milk powder, pet food and animal feed, causing a series of human and animal deaths due to kidney failure, is an important nitrogen-heterocyclic organic chemical raw material, often used in the production of plastics, glue, textiles, etc. , leather, medicine and flame retardants are also used to make fertilizers in some Asian countries. At the same time, melamine is also a metabolite of a pesticide called cyromazine. Melamine is closely related to people's lives, and its bi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 孙明星赵雨薇闵红屠虹任盼盼
Owner 上海出入境检验检疫局工业品与原材料检测技术中心
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