CN105974009B - The detection method of zearalenone in a kind of prepared slices of Chinese crude drugs - Google Patents
The detection method of zearalenone in a kind of prepared slices of Chinese crude drugs Download PDFInfo
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- CN105974009B CN105974009B CN201610272135.2A CN201610272135A CN105974009B CN 105974009 B CN105974009 B CN 105974009B CN 201610272135 A CN201610272135 A CN 201610272135A CN 105974009 B CN105974009 B CN 105974009B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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Abstract
The invention discloses a kind of detection methods of zearalenone in prepared slices of Chinese crude drugs, including crush, alkali leaching, cleaning, extract, high performance liquid chromatography detection step.Compared with prior art, the present invention has the following advantages：(1) the method for the invention is by pre-processing the prepared slices of Chinese crude drugs so that fungi wall is crushed, to improve the accuracy of detection；(2) the method for the invention detection aflatoxin is efficient.
Description
Technical field
The invention belongs to analytical chemistry fields, are related to a kind of mycotoxin detection method more particularly to a kind of prepared slices of Chinese crude drugs
The detection method of middle zearalenone.
Background technology
Mycotoxin is mycetogenetic toxic secondary metabolite, and type is various, pollutes crops, food and feeding extensively
Material etc., seriously threatens human health, has caused the extensive concern in the whole world.
Zearalenone (zearalenone, abbreviation ZEA) is also known as F2 toxin, is mainly generated by sickle-like bacteria, is a kind of female
Hormone mycotoxin is widely present in the cereal crops such as the corn to go mouldy, sorghum and milk fish, mainly acts on reproduction
System has stronger genotoxicity and teratogenesis, animal can be caused infertile or miscarried.
Chinese medicine and its associated product category are various, and medicinal material plantation area is extensive, in production, processing, transport, storage process
In, it is easy to it goes mouldy and pollutes various fungies, generate harmful mycotoxin, Chinese medicine mycotoxin pollution problem
Also result in the attention of insider.2001, Department of Commerce of the People's Republic of China (PRC) disclosed《Medicinal plant and preparation foreign trade
Green professional standard》, it is specified that aflatoxin B1 limitation should be less than being equal to 5 μ g/kg.《Chinese Pharmacopoeia》Version one is included within 2010
Aflatoxin B1 in Chinese medicine, B2, G1, the high performance liquid chromatography fluorescence detection method of G2, to peach kernel, the sterculia seed, dried orange peel etc.
Chinese medicine define AFB1 highests limitation be 5 μ g/kg, AF (B1+B2+G1+G2) highests limit the quantity be 10 μ g/kg.Therefore, no matter from guarantor
Hinder Chinese medicine and its safety of Related product or the management aspect of Import and export of Chinese traditional medicines, it is necessary to establish a mycotoxin
The technology platform of more residual contamination detections, further improves the quality control procedure of Chinese medicine and products thereof.But only detection is yellow
The content of aspertoxin, and it is not comprehensive enough not have specific limitation regulation to other toxin.No matter from ensure Chinese medicine and its
The safety of Related product or the management aspect of Import and export of Chinese traditional medicines, it is necessary to establish the more residual contaminations of mycotoxin
The technology platform of detection further improves the quality control procedure of Chinese medicine and products thereof.
The method of the zearalenone detected in the prior art is more, but has the following disadvantages：In detection process
Due to easily being interfered by other toxin, testing result is inaccurate；In addition, testing process is more complex, detection time is extended,
Improve testing cost.
Invention content
Present invention solves the technical problem that being：In order to overcome the defect of the above-mentioned prior art, it is accurate to obtain a kind of testing result
Really, testing process is simple, and the lower method of testing cost, the present invention provides a kind of inspections of zearalenone in prepared slices of Chinese crude drugs
Survey method.
Technical solution：The detection method of zearalenone, comprises the steps of in a kind of prepared slices of Chinese crude drugs：
(1) prepared slices of Chinese crude drugs are added in pulverizer, power is 1.2~1.8kW/h, rotating speed is 2500~3200 revs/min,
Input medicine materical crude slice amount is 2~5kg per hour, and attrition grinding to powdery, powder diameter is 200~400 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 0.5%~2.5% and infiltrates 0.5~3
Hour, with distilled water flushing to neutrality, it is placed in baking oven and is dried under the conditions of 58~75 DEG C；
(3) powder after drying step (2) is extracted with 34~56% methanol of mass concentration, and extracting solution vibrates 13~28 points
Clock centrifuges 5~10 minutes under the conditions of 4 DEG C, 6000~8000 revs/min, takes supernatant；
(4) use high performance liquid chromatography detection step (3) in supernatant, mobile phase be 3~5mol/L ammonium formate with
0.2~0.4% formic acid by volume 1~5:3 mixing, flow velocity are 0.3~0.8mL/min, and column temperature is 25~28 DEG C, sample temperature
Degree is 4~8 DEG C, and sampling volume is 5~10 μ L.
Preferably, the prepared slices of Chinese crude drugs are added in pulverizer in step (1), power 1.6kW/h, rotating speed are 2900 revs/min
Clock, per hour input medicine materical crude slice amount are 4kg, and attrition grinding to powdery, powder diameter is 350 mesh.
Preferably, which is characterized in that the powder that step (1) obtains is placed in the carbon that mass concentration is 1.8% in step (2)
It is infiltrated 2.4 hours in sour sodium, with distilled water flushing to neutrality, is placed in baking oven and is dried under the conditions of 66 DEG C.
Preferably, which is characterized in that the powder after drying step (2) in step (3) is carried with 46% methanol of mass concentration
It takes, extracting solution vibrates 24 minutes, is centrifuged 7 minutes under the conditions of 4 DEG C, 7200 revs/min, takes supernatant.
Preferably, which is characterized in that using the supernatant in high performance liquid chromatography detection step (3), flowing in step (4)
Be mutually 4.2mol/L ammonium formate and 0.3% formic acid by volume 4:3 mixing, flow velocity 0.7mL/min, column temperature are 26 DEG C,
Sample temperature is 5 DEG C, and sampling volume is 6 μ L.
Advantageous effect：(1) detection method of the present invention eliminates other toxin to Gibberella zeae alkene by alkaline cleaning procedure
The interference of ketone detection, improves its accuracy in detection；(2) detection method testing process of the present invention is simple, takes shorter, inspection
It is relatively low to survey cost.
Specific implementation mode
Embodiment 1
The detection method of zearalenone, comprises the steps of in a kind of prepared slices of Chinese crude drugs：
(1) prepared slices of Chinese crude drugs are added in pulverizer, power 1.2kW/h, rotating speed are 2500 revs/min, put into per hour
Medicine materical crude slice amount is 2kg, and attrition grinding to powdery, powder diameter is 200 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 0.5% and is infiltrated 0.5 hour, with distillation
Water is rinsed to neutrality, is placed in baking oven and is dried under the conditions of 58 DEG C；
(3) powder after drying step (2) is extracted with 34% methanol of mass concentration, and extracting solution vibrates 13 minutes, 4
DEG C, centrifuge 5 minutes under the conditions of 6000 revs/min, take supernatant；
(4) use high performance liquid chromatography detection step (3) in supernatant, mobile phase be 3mol/L ammonium formate with
0.2% formic acid by volume 1:3 mixing, flow velocity 0.3mL/min, column temperature are 25 DEG C, and sample temperature is 4 DEG C, sampling volume
For 5 μ L.
Embodiment 2
The detection method of zearalenone, comprises the steps of in a kind of prepared slices of Chinese crude drugs：
(1) prepared slices of Chinese crude drugs are added in pulverizer, power 1.6kW/h, rotating speed are 2900 revs/min, put into per hour
Medicine materical crude slice amount is 4kg, and attrition grinding to powdery, powder diameter is 350 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 1.8% and is infiltrated 2.4 hours, with distillation
Water is rinsed to neutrality, is placed in baking oven and is dried under the conditions of 66 DEG C；
(3) powder after drying step (2) is extracted with 46% methanol of mass concentration, and extracting solution vibrates 24 minutes, 4
DEG C, centrifuge 7 minutes under the conditions of 7200 revs/min, take supernatant；
(4) use high performance liquid chromatography detection step (3) in supernatant, mobile phase be 4.2mol/L ammonium formate with
0.3% formic acid by volume 4:3 mixing, flow velocity 0.7mL/min, column temperature are 26 DEG C, and sample temperature is 5 DEG C, sampling volume
For 6 μ L.
Embodiment 3
The detection method of zearalenone, comprises the steps of in a kind of prepared slices of Chinese crude drugs：
(1) prepared slices of Chinese crude drugs are added in pulverizer, power 1.8kW/h, rotating speed are 3200 revs/min, put into per hour
Medicine materical crude slice amount is 5kg, and attrition grinding to powdery, powder diameter is 400 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 2.5% and is infiltrated 3 hours, use distilled water
It rinses to neutrality, is placed in baking oven and is dried under the conditions of 75 DEG C；
(3) powder after drying step (2) is extracted with 56% methanol of mass concentration, and extracting solution vibrates 28 minutes, 4
DEG C, centrifuge 10 minutes under the conditions of 8000 revs/min, take supernatant；
(4) use high performance liquid chromatography detection step (3) in supernatant, mobile phase be 5mol/L ammonium formate with
0.4% formic acid by volume 5:3 mixing, flow velocity 0.8mL/min, column temperature are 28 DEG C, and sample temperature is 8 DEG C, sampling volume
For 10 μ L.
The zearalenone in the prepared slices of Chinese crude drugs is detected using the detection method described in above-described embodiment 1~3, is tied
Fruit is as shown in the table：
Claims (1)
1. the detection method of zearalenone in a kind of prepared slices of Chinese crude drugs, which is characterized in that comprise the steps of：
（1）The prepared slices of Chinese crude drugs are added in pulverizer, power 1.6kW/h, rotating speed are 2900 revs/min, put into medicine materical crude slice per hour
Amount is 4kg, and attrition grinding to powdery, powder diameter is 350 mesh；
（2）By step（1）The powder of acquisition, which is placed in the sodium carbonate that mass concentration is 1.8%, to be infiltrated 2.4 hours, is rushed with distilled water
It is washed till neutrality, is placed in baking oven and is dried under the conditions of 66 DEG C；
（3）By step（2）Powder after drying is extracted with 46% methanol of mass concentration, and extracting solution vibrates 24 minutes, 4 DEG C, 7200
It is centrifuged 7 minutes under the conditions of rev/min, takes supernatant；
（4）Using high performance liquid chromatography detection step（3）In supernatant, the ammonium formate and 0.3% that mobile phase is 4.2mol/L
Formic acid by volume 4:3 mixing, flow velocity 0.7mL/min, column temperature are 26 DEG C, and sample temperature is 5 DEG C, and sampling volume is 6 μ L.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297903A (en) * | 2010-06-25 | 2011-12-28 | 中国医学科学院药用植物研究所 | A method for detecting zearalenone toxins in traditional Chinese medicines with different matrixes |
| CN102590363A (en) * | 2011-01-05 | 2012-07-18 | 中国医学科学院药用植物研究所 | Method for detecting zearalenone toxin and metabolin alpha-zearalenol toxin thereof in traditional Chinese medicines with different matrixes |
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2016
- 2016-04-28 CN CN201610272135.2A patent/CN105974009B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102297903A (en) * | 2010-06-25 | 2011-12-28 | 中国医学科学院药用植物研究所 | A method for detecting zearalenone toxins in traditional Chinese medicines with different matrixes |
| CN102590363A (en) * | 2011-01-05 | 2012-07-18 | 中国医学科学院药用植物研究所 | Method for detecting zearalenone toxin and metabolin alpha-zearalenol toxin thereof in traditional Chinese medicines with different matrixes |
Non-Patent Citations (3)
| Title |
|---|
| 中药中玉米赤霉烯酮的残留测定;毛丹 等;《齐鲁药事》;20120731;第31卷(第7期);全文 * |
| 中药饮片中黄曲霉毒素和玉米赤霉烯酮的液质联用检测分析;谭婧 等;《时珍国医国药》;20121031;第23卷(第10期);第2469-2472页 * |
| 高效液相色谱-二极管阵列检测器同时测定中药中榆木赤霉烯酮和玉米赤霉烯醇;申红红 等;《中华中医药杂志》;20120531;第27卷(第5期);全文 * |
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