Determination method of benzo(a)pyrene in Camellia oleifera seed oil

A technology of Camellia oleifera seed oil and a detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of large influence of environmental factors, high requirements for neutral alumina, and difficulty in ensuring reproducibility, so as to achieve a small impact on the external environment , the effect of accurate quantitative analysis

Inactive Publication Date: 2011-12-21
RES INST OF SUBTROPICAL FORESTRY CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The national standard measurement method GB/T 5009.27-2003 uses fluorescence spectrophotometry and visual colorimetry, which is greatly affected by environmental factors and is prone to errors caused by external interference; the national standard measurement method GB/T 22509-2008 uses high-efficiency liquid phase-fluorescence detection The instrume

Method used

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  • Determination method of benzo(a)pyrene in Camellia oleifera seed oil
  • Determination method of benzo(a)pyrene in Camellia oleifera seed oil
  • Determination method of benzo(a)pyrene in Camellia oleifera seed oil

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Weigh 1.5g of Camellia oleifera seed oil sample (known to contain 12.0±0.5μg / kg of benzo(a)pyrene) into a 25mL triangular flask, add 90mL of 3mol / L potassium hydroxide ethanol solution, at 75 ℃ water bath condensation reflux saponification 1h;

[0031] 2) Take out the saponification solution and cool it, pour all the saponification solution into a 500mL separatory funnel, add 50mL saturated sodium chloride solution, add petroleum ether (100mL, divided into 3 times), shake vigorously, and extract 3 times;

[0032] 3) Combine the extracts in a 250mL separatory funnel, wash with ultrapure water until neutral, filter the petroleum ether phase through anhydrous sodium sulfate into a 250mL ground-mouth round-bottom flask, and rotate it to dryness in a water bath at 40°C , add 2mL of petroleum ether to obtain the extract, to be purified;

[0033] 4) Activate the neutral alumina purification column (250mg, 3mL) with 5.0mL petroleum ether first, the flow rate is about 2.0mL / ...

Embodiment 2

[0038] 1) Weigh 3g of Camellia oleifera seed oil sample (known to contain 8.0±0.2μg / kg of benzo(a)pyrene) into a 25mL ground-mouth Erlenmeyer flask, add 100mL of 2.5mol / L potassium hydroxide ethanol solution, at 85 ℃ water bath condensation reflux saponification 1.5h;

[0039] 2) Take out the saponification solution and cool it, pour all the saponification solution into a 500mL separatory funnel, add 80mL saturated sodium chloride solution, add petroleum ether (200mL, divided into 3 times), shake vigorously, and extract 3 times;

[0040]3) Combine the extracts in a 250mL separatory funnel, wash with ultrapure water to neutrality, filter the petroleum ether phase through anhydrous sodium sulfate into a 250mL ground-mouth round bottom flask, and rotate it to dryness in a water bath at 35°C , add 3mL of petroleum ether to obtain the extract, to be purified;

[0041] 4) Activate the neutral alumina purification column (250mg, 3mL) with 8.0mL petroleum ether first, the flow rate i...

Embodiment 3

[0046] 1) Weigh 5g of Camellia oleifera seed oil sample (known to contain benzo(a)pyrene 4±0.2μg / kg) into a 25mL grinding mouth Erlenmeyer flask, add 300mL, 1mol / L potassium hydroxide ethanol solution, at 100℃ Condensate in a water bath and reflux for saponification for 2 hours;

[0047] 2) Take out the saponification solution and cool it, pour all the saponification solution into a 500mL separatory funnel, add 100mL saturated sodium chloride solution, add petroleum ether (300mL, divided into 3 times), shake vigorously, and extract 3 times;

[0048] 3) Combine the extracts in a 250mL separatory funnel, wash with ultrapure water until neutral, filter the petroleum ether phase through anhydrous sodium sulfate into a 250mL ground-mouth round-bottom flask, and rotate it to dryness in a water bath at 45°C , add 1mL of petroleum ether to obtain the extract, to be purified;

[0049] 4) Activate the neutral alumina purification column (250mg, 3mL) with 10mL petroleum ether first, the...

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Abstract

The invention discloses a method for detecting benzo(a)pyrene in Camellia oleifera seed oil, belonging to the technical field of food safety detection. It includes steps such as sample extraction, purification and qualitative and quantitative analysis. The invention adopts a stable high-performance liquid chromatography method, is less affected by the external environment, can accurately quantitatively analyze, and has a detection limit of 1 μg/kg. The invention adopts a saponification method to change the properties of the oil matrix, and then purifies it with an alumina purification column, so that a better purification effect can be achieved even if the sampling amount is increased.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and in particular relates to a detection method of benzo(a)pyrene in Camellia oleifera seed oil. Background technique [0002] Benzopyrene is also known as benzo(a)pyrene, English abbreviation BaP, benzo(a)pyrene belongs to polycyclic aromatic hydrocarbons, is a common highly active indirect carcinogen, its chemical properties are stable, and it is not easy to decompose under natural conditions , and has strong fat solubility. Among the more than 400 major carcinogens that have been detected so far, more than half are compounds belonging to the class of polycyclic aromatic hydrocarbons, and benzo(a)pyrene is one of the strong carcinogens. It can cause tumors or cancers in the stomach, esophagus, skin and other parts, and more serious ones can cause deformities and gene mutations. Camellia oleifera seed oil is of good quality and rich in nutrition. Its fatty acid composition is sim...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 汤富彬莫润宏钟冬莲沈丹玉倪张林屈明华
Owner RES INST OF SUBTROPICAL FORESTRY CHINESE ACAD OF FORESTRY
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