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Rapid detection method for cyanide in sorghum

A detection method and cyanide technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of long time, large detection error, cumbersome pretreatment, etc., and achieve the effect of high accuracy, high sensitivity, and difficult judgment.

Pending Publication Date: 2021-06-01
济南趵突泉酿酒有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The detection of cyanide in food adopts GB 5009.36-2016: the first method of spectrophotometry. This method is not suitable for the detection of cyanide content in sorghum, because when extracting cyanide in sorghum, it will also extract cyanide in sorghum. Colored substances such as pigments are extracted, which will cause interference when detected by a spectrophotometer, and the pretreatment is cumbersome, the time is long, and the repeatability is poor; the second method headspace-gas phase Chloramine T derivative chromatography, in acid The cyanide in sorghum is derivatized into cyanogen chloride with chloramine T under the condition of acidity, and the cyanide and the H therein + reaction to generate hydrocyanic acid, but due to the volatilization of hydrocyanic acid, the detection result is low or even the target compound cannot be detected; the third method: qualitative method, this method can only determine the existence of cyanide, but cannot determine the presence of cyanide in sorghum. Specific content of cyanide
[0004] For the detection of cyanide in food, there are existing methods in addition to the national standard method: 1. The headspace gas phase method uses the principle of derivation of brominated water to detect the content of cyanide. However, brominated water in this method has strong oxidizing properties and is volatile. 2. Silver nitrate titration method, which needs to use distillation to extract cyanide, and cyanide is easy to lose during the distillation process, resulting in inaccurate detection results; 3. Ion chromatography detects cyanide, directly Use the amperometric detector to measure the operation method, the detection line is 0.1ppm, when the cyanide content is low, the detection error is large

Method used

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  • Rapid detection method for cyanide in sorghum
  • Rapid detection method for cyanide in sorghum
  • Rapid detection method for cyanide in sorghum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Standard curve and linear relationship

[0046] The method provided in this embodiment includes the following steps:

[0047] (1) Preparation of the solution:

[0048] Cyanide ion standard solution: 1000μg / mL (mother solution);

[0049] Cyanide standard intermediate solution 1μg / mL (prepared and used now): Take 100μL cyanide standard solution and dilute to 100mL with ultrapure water;

[0050] 0.5mol / L phosphate buffer solution: 3.4g anhydrous potassium dihydrogen phosphate and 3.55g anhydrous disodium hydrogen phosphate, dissolved in ultrapure water, and dilute to 100mL;

[0051] 10g / L Chloramine T solution (preparation for current use): Dissolve 1g Chloramine T in ultrapure water and dilute to 100mL;

[0052] (2) Sample pretreatment, the specific process is as follows: sorghum is pulverized into powder with a high-speed universal grinder, and it feels grainy to the touch, and the particle diameter is about 1mm. 10mL of pure water, put the headspace bottle into the ...

Embodiment 2

[0063] Embodiment 2 Precision experiment

[0064] The method provided in this embodiment includes the following steps:

[0065] Take 1 g of the same crushed sorghum sample, and perform three independent repeated measurements according to the steps in Example 1, and the RSD obtained is 3.182%, which is within the range of 5% required by the precision test standard, indicating that the method has high precision. The specific precision test results are shown in Table 1:

[0066] Table 1 Evaluation data of detection method for cyanide content in sorghum

[0067]

[0068]

Embodiment 3

[0069] Embodiment 3 recovery rate experiment

[0070] The method provided in this embodiment includes the following steps:

[0071] Add 10 μg / L, 20 μg / L, and 30 μg / L three different concentrations of cyanide standard substances to the cyanide extract of the same sorghum sample, and measure it according to the steps described in Example 1, and each concentration is repeated under repeated conditions. The recovery rate was determined twice independently, and the recovery rate was in the range of 89.5-108.9, indicating that the performance of the method met the requirements. The specific recovery rate experimental results are shown in Table 2:

[0072] Table 2 Evaluation data of cyanide content detection method (cyanide concentration in headspace vial) in sorghum

[0073]

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Abstract

The invention belongs to the field of food analysis, and provides a rapid detection method of cyanide in sorghum. The method comprises the following steps of: directly adding a crushed sample into a headspace sample introduction bottle; ultrasonically extracting cyanide in sorghum by using ultrapure water; performing still standing in an ice-water bath for 5 minutes; adding a phosphate buffer solution and chloramine T under the condition of the ice-water bath, immediately performing covering and uniformly mixing; performing detection through gas chromatography-headspace chromatography, adopting a sample injection mode with the split ratio being 50: 1; performing quantification through using a standard curve method; and finally, calculating the content of the cyanide in the sorghum. According to the method, a chromatographic column used for gas chromatography-headspace chromatography detection is an HP-5 chromatographic column, and the specification of the chromatographic column is 30 m*0.32 mm*0.25 mu m; and a detection result shows that R2 is equal to 0.999, the recovery rate is 89.5%-108.9%, the precision RSD is equal to 3.182%, and the detection limit is 3 [mu] g / L. The detection method has the advantages of good reproducibility, high precision and high sensitivity, and is suitable for detecting cyanide in sorghum.

Description

technical field [0001] The invention belongs to the technical field of food analysis and detection, and provides a rapid detection method for cyanide in sorghum. Background technique [0002] The national standard 2757-2012 requires that the content of cyanide (calculated as HCN) in distilled liquor should not exceed 8.0mg / L. If sorghum is used as the main raw material for brewing, after fermentation, some cyanide in the fermented grains will enter the liquor with distillation, thus affecting the content of cyanide in liquor, so how to quickly detect the content of cyanide in sorghum to screen cyanide Cyanide sorghum varieties with low cyanide content play an important role in reducing the cyanide content in liquor. [0003] The detection of cyanide in food adopts GB 5009.36-2016: the first method of spectrophotometry. This method is not suitable for the detection of cyanide content in sorghum, because when extracting cyanide in sorghum, it will also extract cyanide in sorg...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/24G01N30/86G01N30/60
CPCG01N30/02G01N30/06G01N30/24G01N30/8634G01N30/6052G01N2030/067
Inventor 吕志远秦炳伟苏宁卢春玲韩云翠邱振清李强马春莲
Owner 济南趵突泉酿酒有限责任公司
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