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Detection method of sodium copper chlorophyll in olive oil by liquid chromatography tandem mass spectrometer (lc-ms/ms)

A copper chlorophyllin sodium and liquid chromatography technology, which is applied in the field of food additive detection, can solve the problems of low copper chlorophyllin sodium content and difficult detection, and achieve the effect of low detection limit

Inactive Publication Date: 2016-09-07
镇江出入境检验检疫局检验检疫综合技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sodium copper chlorophyllin added to soybean oil or other oils has a low content, and it is difficult to detect by the current spectrophotometric method. Therefore, a more reliable, accurate, and high-sensitivity method is needed to qualitatively and quantitatively detect the content of this substance in oils and fats. exist

Method used

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  • Detection method of sodium copper chlorophyll in olive oil by liquid chromatography tandem mass spectrometer (lc-ms/ms)
  • Detection method of sodium copper chlorophyll in olive oil by liquid chromatography tandem mass spectrometer (lc-ms/ms)
  • Detection method of sodium copper chlorophyll in olive oil by liquid chromatography tandem mass spectrometer (lc-ms/ms)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] standard curve drawing

[0037] 1. Preparation of sodium copper chlorophyllin standard solution

[0038] Weigh 6.4 mg of sodium copper chlorophyllin standard substance into a 50mL brown volumetric flask, add aqueous methanol solution, dilute to constant volume to obtain a standard stock solution with a sodium copper chlorophyllin content of 128.0 mg / L; then draw 1.0mL of the stock solution into a 100mL capacity In the bottle, methanol aqueous solution was added to constant volume to prepare a standard working solution of sodium copper chlorophyllin with a sodium copper chlorophyllin content of 1.28 mg / L. Store the standard working solution at 4°C.

[0039] Based on the standard working solution prepared above, dilute it with a methanol-water mixed solution to obtain the required concentration of the standard solution. In this embodiment, prepare 7 standard solutions with different concentrations: add 1.0 mL of methanol aqueous solution, accurately absorb 1.0mL copper ...

Embodiment 2

[0046] Sample pretreatment

[0047]Accurately weigh 0.700 g of olive oil sample, accurately add 2 mL of methanol-water mixed solution, in which methanol accounts for 80% by volume, and mix well. Add ether 3mL and mix well. Centrifuge at 5000 rpm for 20 minutes at 20°C. Take the water phase layer and pass through the water phase membrane; accurately draw 10uL and directly inject the sample into the liquid chromatography tandem mass spectrometer for detection

[0048] The liquid chromatography tandem mass spectrometry detection method is the same as the above-mentioned chromatography mass spectrometry detection conditions: electrospray ionization source (ESI), scanning mode is positive ion; spray voltage 4000V; transmission capillary temperature 350°C; shell gas pressure 20arb; multiple reaction monitoring ( SRM); chromatographic column: Agilent ZORBAX XDB-C18 (3.5 um, 2.1×50mm); column temperature: room temperature; injection volume 10uL; mobile phase preparation: organic pha...

Embodiment 3

[0051] Spike experiment 1

[0052] Accurately weigh 0.700g of the above-mentioned negative olive oil sample, absorb 23.4uL of the 1.28mg / L sodium copper chlorophyllin standard working solution prepared above, add it and mix evenly, accurately add 2.0mL of methanol-water mixed solution, and mix evenly; among them, methanol-water mixed solution , by volume percentage, methanol accounted for 80%, water accounted for 20%; add ether 4mL, mix well. Centrifuge at 20°C and 5000rpm for 20 minutes. Take the water phase layer to pass through the water phase membrane, and directly inject it into the liquid chromatography mass spectrometer for detection. The detection conditions of liquid chromatography mass spectrometry are the same as above, electrospray ionization source (ESI), scan mode is positive ion; spray voltage 4000V; transfer capillary temperature 350°C; shell gas pressure 20arb; multiple reaction monitoring (SRM); chromatographic column: Agilent ZORBAX XDB-C18 (3.5 um, 2.1×50...

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Abstract

The invention provides a method detecting sodium copper chlorophyllin in olive oil through an LC-MS / MS (liquid chromatography-tandem mass spectrometer). The method comprises the following steps: (1) preprocessing a sample; and (2) qualitatively and quantitatively detecting chromatograph and mass spectrometry conditions of sodium copper chlorophyllin by the LC-MS / MS, and feeding at the constant flowing speed of 250microliter / min, wherein the water phase of a mobile phase is a 5-20mmoL / L ammonium acetate water solution, the organic phase is methyl alcohol, and the mobile phase comprises the following components in percentage by volume: 80% to 100% of methyl alcohol, and 0 to 20% of the ammonium acetate water solution; and detecting that the parent ions are 613.3m / z, the quantitative daughter ions are 465.6m / z, the collision energy is 56V, the qualitative daughter ions are 479.9m / z, and the collision energy is 38V. With the adoption of the method, sodium copper chlorophyllin in olive oil can be accurately, reliably, qualitatively and quantitatively detected with high sensitivity.

Description

technical field [0001] The invention relates to the field of food additive detection, in particular to the detection of sodium copper chlorophyllin illegally added in olive oil. Background technique [0002] As a food additive, sodium copper chlorophyllin is allowed to be used as a coloring agent in frozen drinks, canned vegetables, cooked beans, processed nuts, candies, baked goods, fruit and vegetable juices, prepared wine, etc., and the content shall not exceed 500ppm. But sodium copper chlorophyllin is forbidden in oil. In the domestic and foreign literature and testing standards, the current methods for the determination of sodium copper chlorophyllin are very limited, and most methods use spectrophotometry (such as GB / T23749-2009). Since sodium copper chlorophyllin is a food additive allowed in GB2760, its addition amount is relatively large, and the maximum limit is 500ppm. These detection methods are mainly to detect its content, and the limit of quantification is r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 周洪斌李平肖震陈桐
Owner 镇江出入境检验检疫局检验检疫综合技术中心
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