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High performance liquid chromatographic method for detecting mass concentration of sodium sulfocyanate in milk and dairy product

A high-performance liquid chromatography, sodium thiocyanate technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of complex treatment methods and impact on recovery rate, and achieve good adsorption effect, good accuracy, and high detection sensitivity. Effect

Inactive Publication Date: 2016-04-20
青岛市动物疫病预防控制中心
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used detection method for sodium thiocyanate in milk and dairy products is ion chromatography, which has the characteristics of high sensitivity and good separation effect, but its pretreatment method is complicated and the recovery rate is also affected

Method used

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  • High performance liquid chromatographic method for detecting mass concentration of sodium sulfocyanate in milk and dairy product
  • High performance liquid chromatographic method for detecting mass concentration of sodium sulfocyanate in milk and dairy product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Pretreatment steps of milk and dairy products: first add 5ml of acetonitrile to 10ml of milk sample, and precipitate to remove the protein in the milk sample. Then a solid-phase extraction column is used to remove part of the water-soluble vitamins and amino acids in the milk or dairy product sample, and the eluate is collected. The solid-phase extraction column uses basic alumina as a filler. Then the eluate was centrifuged and degreased, and it was ready to be detected by high performance liquid chromatography.

[0029] Determine the chromatographic conditions as follows: mobile phase is 0.2% triethylamine phosphate (pH=7.0): acetonitrile=95: 5, in volume ratio; 0.2% triethylamine sulfate is prepared as follows: first dissolve phosphoric acid in deionized water Prepare a phosphoric acid solution with a mass concentration of 0.2%, and then add triethylamine to the phosphoric acid solution to adjust the pH to 7. Agela-ASBCl8 (250mm×4.6mm, 5μm) chromatographic column; c...

Embodiment 2

[0031] The pretreatment steps of milk and dairy products are the same as in Example 1.

[0032] Determine the chromatographic conditions as follows: mobile phase is 0.2% triethylamine phosphate (pH=7.0): acetonitrile=95: 5, in volume ratio; 0.2% triethylamine sulfate is prepared as follows: first dissolve phosphoric acid in deionized water Prepare a phosphoric acid solution with a mass concentration of 0.2%, and then add triethylamine to the phosphoric acid solution to adjust the pH to 7. Agela-ASBCl8 (250mm×4.6mm, 5μm) chromatographic column; column temperature is 25°C; flow rate is controlled at 0.8mL / min; detection wavelength is 215nm; injection volume is 9μL. Under the above chromatographic conditions, the system suitability test was carried out on the blank, standard working solution and sample solution. The theoretical plate of sodium thiocyanate was 7623, the separation between the main peak and the impurity peak was greater than 2.0, and the tailing factor was 1.25. A...

Embodiment 3

[0034] The pretreatment steps of milk and dairy products are the same as in Example 1.

[0035] Determine that the chromatographic conditions are: mobile phase is 0.2% triethylamine phosphate (pH=7.0): acetonitrile=95: 5; Agela-ASBCl8 (250mm * 4.6mm, 5 μ m) chromatographic column; Column temperature is 30 ℃; Flow velocity is controlled at 0.8mL / min; the detection wavelength is 218nm; the injection volume is 10μL. Under the above chromatographic conditions, the system suitability test was carried out on the blank, standard working solution and sample solution. The theoretical plate of sodium thiocyanate was 7623, the separation between the main peak and the impurity peak was greater than 2.0, and the tailing factor was 1.25. According to the calculation of 3 times the signal-to-noise ratio, the detection limit can be 1 mg / L, and the 10-fold signal-to-noise ratio can be used to calculate the limit of quantification to be 3.3 mg / L. The detection limit can reach 0.2 mg / kg; the me...

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Abstract

The invention discloses a high performance liquid chromatographic method for detecting the mass concentration of sodium sulfocyanate in milk and a dairy product. The method comprises the following steps: adding acetonitrile in the a milk or dairy product sample, precipitating to remove protein from the milk or dairy product sample, removing part of water-soluble vitamin and amino-acid with a solid phase extraction column, collecting an eluent, and conducting centrifugal degrease on the eluent to obtain a semi-product for standby use; determining chromatographic conditions as follows: a chromatographic column is an Agela-ASB C18 chromatographic column, column temperature is 25 to 30 DEG C, flow velocity is controlled to be 0.8 mL / min, detection wavelength is 200 to 218 nm, and the sampling quantity is 8 to 10 [mu]m. The high performance liquid chromatographic method is based on a reversed-phase ion-pair chromatographic method, and is simple in pretreatment, high in detection sensitivity, good in accuracy, stable in result, and wide in popularization.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography method for measuring the mass concentration of sodium thiocyanate in milk and dairy products, and belongs to the technical field of quality and safety detection of milk and dairy products. Background technique [0002] Sodium thiocyanate is a poisonous chemical raw material, and the state prohibits its addition and use in food processing. Unscrupulous traders add it to milk and dairy products to keep fresh. At present, the commonly used detection method for sodium thiocyanate in milk and dairy products is ion chromatography, which has the characteristics of high sensitivity and good separation effect, but its pretreatment method is complicated and the recovery rate is also affected. Contents of the invention [0003] The object of the present invention is to provide a kind of high performance liquid chromatography method of measuring the mass concentration of sodium thiocyanate in mil...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/89
CPCG01N30/02G01N30/89G01N2030/027
Inventor 李彦付红蕾吴燕李辉穆阿丽庄桂玉
Owner 青岛市动物疫病预防控制中心
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