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Method for detecting paraffin content in food and pretreatment method of paraffin samples

A sample pretreatment and paraffin technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of being easily affected by solvents and other factors, cumbersome quantitative procedures, excessive water or solvents, etc., and achieve low toxicity and quantitative results Accurate, low temperature effect

Inactive Publication Date: 2012-09-12
GUANGZHOU QUALITY SUPERVISION & TESTING INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Detection of Solid Paraffin in Hot Pot Bottom by Fourier Transform Infrared Spectroscopy" In the sample pretreatment process, hot water was added to quickly freeze the extracted fat layer for saponification and impurity removal, but the quantitative procedure is cumbersome, and more solids may be produced during the saponification process substances, more water or solvents are needed, and in view of the fact that fingerprints in the field of fingerprints are one of the characteristics of infrared spectroscopy, they are easily affected by solvents and other factors, and the interference of impurities is significant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 detects the paraffin content in the chafing dish bottom material

[0030] Proceed as follows:

[0031] (1) Sampling

[0032] Stir the hot pot bottom material evenly, take 9 parallel samples, and weigh 5g (accurate to 0.001g) for each sample; add 0.5ml of paraffin standard solution with a concentration of 100μg / ml to 3 samples.

[0033] All samples were subjected to sample pretreatment as follows:

[0034] (2) Leaching

[0035] First add 20ml of cyclohexane, ultrasonically extract for 30min, centrifuge at 2500r / min for 5min, collect the supernatant, repeat the extraction twice, combine the cyclohexane extract and dilute to 40ml for later use;

[0036] (3) oxidation

[0037] Take 1.0ml of the extract of step (2), add 1.0ml of oxidizing reagent, the oxidizing reagent is a compound solution of 1g of chromium trioxide: 1ml of concentrated sulfuric acid: 2ml of water, shake and react for 30min;

[0038] (4) Centrifugal separation

[0039] Add 5ml of cyclohe...

Embodiment 2

[0049] Embodiment 2 detects the paraffin content in the chafing dish bottom material

[0050] Proceed as follows:

[0051] (1) Sampling

[0052] Stir the hot pot bottom material evenly, take 9 parallel samples, and weigh 5g (accurate to 0.001g) for each sample; add 0.5ml of paraffin standard solution with a concentration of 100μg / ml to 3 samples.

[0053] All samples were subjected to sample pretreatment as follows:

[0054] (2) Leaching

[0055] First add 20ml of cyclohexane, ultrasonically extract for 5min, centrifuge at 2500r / min for 5min, collect the supernatant, repeat the extraction for 2 times, combine the cyclohexane extract and dilute to 40ml for later use;

[0056] (3) oxidation

[0057] Take 1.0ml of the extract of step (2), add 1.0ml of oxidizing reagent, the oxidizing reagent is a compound solution of 1g of chromium trioxide: 1ml of concentrated sulfuric acid: 2ml of water, shake and react for 30min;

[0058] (4) Centrifugal separation

[0059] Add 5ml of cy...

Embodiment 3

[0069] Embodiment 3 detects the paraffin content in dried shiitake mushrooms

[0070] Proceed as follows:

[0071] (1) Sampling

[0072] Grind dried shiitake mushrooms into powder, take 9 parallel samples, and weigh 1 g (accurate to 0.001 g) for each sample; add 0.5 ml of paraffin standard solution with a concentration of 100 μg / ml to 3 samples.

[0073] All samples were pretreated as follows:

[0074] (2) Leaching

[0075] First add 5ml of cyclohexane, ultrasonically extract for 10min, centrifuge at 2500r / min for 5min, collect the supernatant, repeat the extraction twice, combine the cyclohexane extract and dilute to 10ml for later use;

[0076] (3) oxidation

[0077] Take 1.0ml of the extract from step (2), add 1.0ml of oxidizing agent, the oxidizing agent is 1g of chromium trioxide: 1ml of concentrated sulfuric acid: 2mL of water compound solution, and shake for 30min;

[0078] (4) Centrifugal separation

[0079] Add 5ml of cyclohexane, shake and extract for 0.5-1min,...

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PUM

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Abstract

The invention discloses a method for detecting paraffin content in food and a pretreatment method of paraffin samples. The pretreatment method includes: sampling, ultrasonic extraction, oxidization, centrifugal separation, column chromatography purification and nitrogen flushing for metering volume. Paraffin content in obtained samples is detected in a gas chromatography or gas chromatography-mass spectrometry method. The pretreatment method of paraffin samples is simple, lass of the samples in pretreatment is little, quantitative results are accurate and recovery rate is high. By adopting the pretreatment method, a plurality of samples can be treated in one time, and batch pretreatment greatly improves work efficiency. Temperature is low and use amount of organic solvents is small so that the operation process if low in toxicity. The pretreatment method is suitable for various food matrixes, small in matrix interference and good in popularization adaptability, and the samples through pretreatment can be used for paraffin content detection in the gas chromatography or gas chromatography-mass spectrometry method.

Description

technical field [0001] The invention relates to a method for detecting paraffin content in food and a sample pretreatment method thereof. Background technique [0002] Paraffin wax is a petroleum product, mainly composed of n-alkanes CnH2n+2 (n=14~34) with different carbon atoms, which is a non-edible substance, which contains heavy metals, benzene, toluene, benzopyrene, long-carbon paraffins, etc. . Excessive consumption of paraffin will reduce immune function, and some substances will accumulate in the human body for a long time, and it will also cause human cell mutation diseases, seriously endangering health. Because paraffin wax is allowed to be used in a small range in the national standard GB2760, quality inspectors will not regard it as a must-check item in food, so paraffin wax has great concealment. In recent years, incidents of paraffin wax being abused in various foods have occurred from time to time, such as polishing in rice, melon seeds and other products to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02
Inventor 罗东辉冼燕萍刘春生陈立伟罗海英侯向昶吴玉銮吴文海
Owner GUANGZHOU QUALITY SUPERVISION & TESTING INST
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