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Method for detecting hypophosphite in flour and flour improvers

A technology of flour improver and hypophosphite, which is applied in the field of analysis and detection, and achieves the effects of simple pretreatment, high accuracy, and good economic and social benefits

Active Publication Date: 2014-11-12
GUANGZHOU QUALITY SUPERVISION & TESTING INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no method for the determination of hypophosphite in food in my country. In order to urge flour production and processing enterprises to produce according to law and ensure the health and safety of the people, it is urgent to develop a method for the determination of hypophosphite in flour and flour improvers.

Method used

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  • Method for detecting hypophosphite in flour and flour improvers
  • Method for detecting hypophosphite in flour and flour improvers
  • Method for detecting hypophosphite in flour and flour improvers

Examples

Experimental program
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Effect test

preparation example Construction

[0041] (2) preparation of need testing solution

[0042] Take flour or flour improver samples and add ethanol water solution with a volume concentration of 70-80% (preferably 75%), ultrasonically extract (extract 20-30min at normal temperature), centrifuge (800-1200r / min centrifuge 3-5min) and take Supernatant, obtain need testing solution after filtering with microporous membrane (filter element size is 0.22 μm);

[0043] (3) Determination

[0044] Precisely absorb the standard solution and inject it into the ultra-high performance liquid chromatography tandem mass spectrometer for determination, and draw a standard curve according to the test results;

[0045] Precisely absorb the test solution and inject it into an ultra-high performance liquid chromatography tandem mass spectrometer for determination, to obtain final product;

[0046] Wherein the chromatographic conditions are: the chromatographic column is SynergiMAX-RP; the column temperature is room temperature; the m...

Embodiment 1

[0051] The mensuration of embodiment 1 hypophosphite standard substance

[0052] 1. Preparation of hypophosphite standard solution: Accurately weigh 100mg of sodium hypophosphite standard product in a 10mL volumetric flask, dilute to the mark with water, shake well, and prepare a concentration of 10.0mg / mL hypophosphite standard product solution, 4 ℃ and protected from light.

[0053] 2. Chromatography and mass spectrometry conditions

[0054] 1) Chromatographic conditions

[0055] Chromatographic column: SynergiMAX-RP4u250×4.6mm, or equivalent;

[0056] Column temperature: room temperature;

[0057] Mobile phase: acetonitrile: 10mmoL / L ammonium acetate solution = 15: 85 (V / V);

[0058] Flow rate: 0.5mL / min, for isocratic elution;

[0059] 2) Mass spectrometry conditions

[0060] Ion source: electrospray ion source (ESI);

[0061] Scanning method: negative ion scanning;

[0062] Capillary voltage: 0.5kV;

[0063] Cone voltage: 30V;

[0064] Ion source temperature: 15...

Embodiment 2

[0075] Determination of hypophosphite content in negative wheat flour of embodiment 2

[0076] 1. Preparation of test solution

[0077] Take 1g of wheat flour sample, add 20mL of 75% (V / V) ethanol aqueous solution (ethanol: water = 3:1), ultrasonically extract at 20°C for 20min, centrifuge at 1000r / min for 3min, take 1mL of supernatant and filter it with microporous Membrane filtration, the filtrate was tested by ultra-high performance liquid chromatography tandem mass spectrometer.

[0078] 2. Chromatographic conditions

[0079] With embodiment 1.

[0080] 3. Draw a standard curve

[0081] The standard curve of Example 1 was used.

[0082] Four. Determination

[0083] Precisely draw 10 μL of the test solution and inject it into the liquid chromatograph, measure it according to the ultra-high performance liquid chromatography tandem mass spectrometry method, and obtain the ultra high performance liquid chromatography tandem mass spectrogram, as shown in the attached ima...

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Abstract

The invention discloses a method for detecting hypophosphite in flour and flour improvers. Super high performance liquid chromatography tandem mass spectrometric detection is adopted by the method. The method comprises the following steps: (1) preparing a standard solution of hypophosphite; (2) preparing a test solution; and (3) measuring, namely precisely sucking the standard solution, injecting the sucked standard solution into a super high performance liquid chromatography tandem mass spectrometer for measurement, drawing a standard curve according to the test result, precisely sucking the test solution and injecting the sucked test solution into the super high performance liquid chromatography tandem mass spectrometer for measurement, thereby obtaining the content of hypophosphite. Inorganic salt (namely hypophosphite) in flour and flour improvers is detected by the super high performance liquid chromatography tandem mass spectrum analyzer, and the detection method is simple in pretreatment and high in accuracy and is suitable for batch detection on hypophosphite in flour and flour improvers.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for detecting hypophosphite in flour and flour improvers. Background technique [0002] my country is the largest wheat producing country in the world. Flour processed from wheat is one of the most important foods for human beings. Flour is the most important raw material for noodle processing, and its quality directly affects the quality of noodle products. With the rapid development of my country's food industry and the improvement of people's living standards, the baking industry has put forward higher requirements for its basic raw material flour. General-purpose flour can no longer meet people's living needs, and the market share of special flour is increasing. rise sharply. Adding appropriate improvers to flour plays an extremely important role in the preparation of modern special flour and the production of flour products. Flour improvers are some ...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 吴玉銮罗海英王斌冼燕萍陈立伟王莉董浩韩婉清黄宇锋
Owner GUANGZHOU QUALITY SUPERVISION & TESTING INST