Sample pretreatment method and determination method for detecting polycyclic aromatic hydrocarbon marker in traditional Chinese medicine product

A technology for sample pretreatment and polycyclic aromatic hydrocarbons, which is applied in the field of analytical chemistry and can solve problems such as large errors

Active Publication Date: 2020-06-16
ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are no standard determination methods and limit requirements for polycyclic aromatic hydrocarbons in Chinese herbal medicines and traditional Chinese medicine extracts, and traditional Chinese medicine health food. Chromatography-mass spectrometry (GC-MS) is used to determine polycyclic aromatic hydrocarbons in food, but due to the complexity of the matrix of traditional Chinese medicine products, this standard is used to detect polycyclic aromatic hydrocarbons in traditional Chinese medicine products, and the error is relatively large

Method used

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  • Sample pretreatment method and determination method for detecting polycyclic aromatic hydrocarbon marker in traditional Chinese medicine product
  • Sample pretreatment method and determination method for detecting polycyclic aromatic hydrocarbon marker in traditional Chinese medicine product
  • Sample pretreatment method and determination method for detecting polycyclic aromatic hydrocarbon marker in traditional Chinese medicine product

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] blank experiment

[0106] Before the experiment, the glassware used was baked at a high temperature of 300°C, and the others were all disposable containers;

[0107] 1) Add 50 μL of D 12 -PAH4 mixed internal standard solution (D 12 -BaA, D 12 -CHR,D 12 -BbFA and D 12 - the concentration of BaP is preferably 0.2 μg / mL) and 10 mL of absolute ethanol are mixed, and the power is 200 W and the frequency is 40 kHz, and ultrasonic extraction is carried out for 5 minutes to obtain the first mixed solution;

[0108] The first mixed solution was mixed with 10 mL of water, then vortex extracted for 1 min at a rotational speed of 2500 rpm, and then ultrasonically extracted for 5 min at a power of 200 W and a frequency of 40 kHz to obtain a second mixed solution;

[0109] After mixing the second mixed solution and 10 mL of n-hexane, the second vortex extraction was carried out at a speed of 2500 rpm for 5 minutes, and then centrifuged at 10000 rpm for 3 minutes, and the superna...

Embodiment 2

[0125] Transfer 0.2mL PAH4 mixed standard solution (concentrations of BaA, CHR, BbFA and BaP are all 0.2 μg / mL) to a 10mL volumetric flask, and dilute to 10mL with acetone to obtain PAH4 mixed standard solution (BaA, CHR, The concentrations of BbFA and BaP are both 0.2 μg / mL);

[0126] 0.02mL of D 12 -PAH4 mixed standard solution (D 12 -BaA, D 12 -CHR,D 12 -BbFA and D 12 - the concentration of BaP is 100.0μg / mL) transferred to the volumetric flask, and the volume was fixed to 10.0mL with acetone to obtain D 12 -PAH4 mixed internal standard solution (D 12 -BaA, D 12 -CHR,D 12 -BbFA and D 12 - the concentration of BaP is 0.2 μg / mL);

[0127] Transfer 5 μL, 10 μL, 25 μL, 50 μL and 100 μL of the PAH4 mixed standard solution to be tested to 5 injection bottles, and add 50 μL of the D 12 -PAH4 mixed internal standard solution, with acetone-isooctane solution (the volume ratio of acetone and isooctane in the acetone-isooctane solution is 1:1) to 200 μ L, to obtain standard ...

Embodiment 3

[0140] Before the experiment, the glassware used was baked at a high temperature of 300 °C;

[0141] 1) Extraction:

[0142] Weigh 1.0 g of the sample to be tested, add 50 μL of 0.2 μg / mL polycyclic aromatic hydrocarbon mixed internal standard solution, add 10 mL of absolute ethanol, and perform ultrasonic extraction for 5 min under the condition of power of 200 W and frequency of 40 kHz to obtain the first mixed solution;

[0143] The first mixed solution was mixed with 10 mL of water, then vortex extracted for 1 min at a rotational speed of 2500 rpm, and then ultrasonically extracted for 5 min at a power of 200 W and a frequency of 40 kHz to obtain a second mixed solution;

[0144] After mixing the second mixed solution and 10 mL of n-hexane, the second vortex extraction was carried out at a speed of 2500 rpm for 5 minutes, and then centrifuged at 10000 rpm for 3 minutes, and the supernatant was taken to obtain the first n-hexane extract;

[0145] 2) purification

[0146] ...

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to a sample pretreatment method and a determination method for detecting a polycyclic aromatic hydrocarbon marker in a traditional Chinese medicine product. The method includes: firstly mixing a to-be-detected sample with ethanol and water, fully wetting and dispersing the to-be-detected sample, and conducting further extraction; selecting n-hexane as an extracting agent to effectively extract benzo[a]anthracene, benzo[b]fluoranthene and benzo[a]pyrene in the to-be-detected sample, and extracting a minimum amount of interfering substance to obtain a first n-hexane extraction solution; then sequentially carrying out Florisil column purification and EU polycyclic aromatic hydrocarbon solid phase extraction column purification on the first n-hexane extraction solution to remove phenolic compounds, chlorophyll, lutein, alkane, fat, yellow pigment and other interfering substances, and removing thesolvent of the obtained purified liquid, thus obtaining a second purified extract, which can be used for precisely detecting the content of the polycyclic aromatic hydrocarbon marker.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a sample pretreatment method and a measurement method for detecting polycyclic aromatic hydrocarbon markers in traditional Chinese medicine products. Background technique [0002] The use of raw materials of Chinese medicinal materials and their extracts in health food is a feature of health food in my country. The National Health and Family Planning Commission has released more than 100 raw materials of traditional Chinese medicine with the same source of medicine and food, but the safety of raw materials of Chinese medicinal materials and their extracts in health food cannot be ignored. In addition to the endogenous toxicity of Chinese herbal medicines, external pollutants such as heavy metals, pesticide residues, mycotoxins, organic pollutants, etc. should also be taken seriously. At present, the production and quality standard system of traditional Chi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/14
CPCG01N30/88G01N30/06G01N30/14G01N2030/065G01N2030/062G01N2030/143
Inventor 吴平谷
Owner ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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