CN105974009A - Detection method of zearalenone in traditional Chinese medicine decoction pieces - Google Patents
Detection method of zearalenone in traditional Chinese medicine decoction pieces Download PDFInfo
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- CN105974009A CN105974009A CN201610272135.2A CN201610272135A CN105974009A CN 105974009 A CN105974009 A CN 105974009A CN 201610272135 A CN201610272135 A CN 201610272135A CN 105974009 A CN105974009 A CN 105974009A
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- 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
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- 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
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- G01N2030/027—Liquid chromatography
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Abstract
The invention discloses a detection method of zearalenone in traditional Chinese medicine decoction pieces, wherein the method comprises the steps of crushing, alkaline leaching, cleaning, extraction and high performance liquid chromatography detection. Compared with the prior art, the detection method has the following advantages: (1) the traditional Chinese medicine decoction pieces are pre-treated by the method, so that fungal walls are broken, so as to improve the accuracy of detection; and (2) the aflatoxin detection efficiency of the method is high.
Description
Technical field
The invention belongs to analytical chemistry field, relate to a kind of mycotoxin detection method, particularly relate to Semen Maydis in a kind of prepared slices of Chinese crude drugs
The detection method of zeranol.
Background technology
Mycotoxin is mycetogenetic poisonous secondary metabolite, of a great variety, extensively pollutes crops, food and feedstuff etc.,
Human health in serious threat, has caused the extensive concern in the whole world.
6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone (zearalenone is called for short ZEA), also known as F2 toxin, is mainly produced by Fusarium spp., is a kind of female sharp
Element mycotoxin, is widely present in the cereal crops such as the Semen Maydis, the Sorghum vulgare Pers. that go mouldy and milk fish, mainly acts on system genitale
System, has stronger genotoxicity and teratogenesis, animal can be caused infertile or miscarriage.
Chinese medicine and associated product category thereof are various, medical material plantation area extensively, producing, process, transport, in storage process,
Being easy to go mouldy and pollute various fungus, produce harmful mycotoxin, Chinese medicine mycotoxin pollution problem is also drawn
Play the attention of insider.Calendar year 2001, Department of Commerce of the People's Republic of China (PRC) discloses " medicinal plants and preparation foreign trade green
Industry standard ", it is stipulated that AFB1 limitation should be less than equal to 5 μ g/kg." Chinese Pharmacopoeia " version one in 2010 is included
AFB1 in Chinese medicine, the high performance liquid chromatography fluorescence detection method of B2, G1, G2, to Semen Persicae, Semen Sterculiae Lychnophorae, Pericarpium Citri Reticulatae
Defining the highest limitation of AFB1 in Chinese medicine is 5 μ g/kg, and AF (B1+B2+G1+G2) the highest limitation is 10 μ g/kg.Cause
This, is no matter from ensureing Chinese medicine and the safety of Related product thereof, or the management aspect of Import and export of Chinese traditional medicines, all it is necessary to set up one
The technology platform of individual mycotoxin many residual contaminations detection, improves the quality control procedure of Chinese medicine and products thereof further.But,
Only detect the content of aflatoxin, and not having concrete limitation regulation to other toxin is the most comprehensive.No matter from guarantee
How residual Chinese medicine and the safety of Related product thereof, or the management aspect of Import and export of Chinese traditional medicines, be all necessary to set up a mycotoxin
Stay the technology platform of pollution detection, improve the quality control procedure of Chinese medicine and products thereof further.
In prior art, the method for the 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone of detection is more, but has the disadvantage that during detection due to easily
Being disturbed by other toxin, therefore testing result is inaccurate；Additionally, testing process is more complicated, extend the detection time, improve
Testing cost.
Summary of the invention
Present invention solves the technical problem that and be: in order to overcome the defect of above-mentioned prior art, it is thus achieved that a kind of testing result is accurate, inspection
Flow gauge is simple, and the method that testing cost is relatively low the invention provides the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs.
Technical scheme: the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs, comprises the steps of
(1) adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.2～1.8kW/h, rotating speed is 2500～3200 revs/min, every
Hour input decoction pieces amount is 2～5kg, 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% infiltration 0.5～3 hour,
With distilled water flushing to neutral, it is placed in baking oven under the conditions of 58～75 DEG C drying；
(3) powder mass concentration 34～56% methanol extraction after step (2) being dried, extracting solution vibrates 13～28 minutes,
At 4 DEG C, under the conditions of 6000～8000 revs/min centrifugal 5～10 minutes, take supernatant；
(4) use the supernatant in high performance liquid chromatography detecting step (3), flowing be mutually 3～5mol/L ammonium formate and 0.2～
The formic acid of 0.4% by volume 1～5:3 mixing, flow velocity is 0.3～0.8mL/min, and column temperature is 25～28 DEG C, sample temperature be 4～
8 DEG C, sampling volume is 5～10 μ L.
Preferably, the prepared slices of Chinese crude drugs are added in pulverizer in (1) by step, power is 1.6kW/h, rotating speed is 2900 revs/min,
Putting into decoction pieces amount per hour is 4kg, and attrition grinding to powdery, powder diameter is 350 mesh.
Preferably, it is characterised in that the powder that step (1) obtains is placed in the carbonic acid that mass concentration is 1.8% by step (2)
Sodium infiltrates 2.4 hours, with distilled water flushing to neutral, is placed in baking oven under the conditions of 66 DEG C drying.
Preferably, it is characterised in that powder mass concentration 46% methanol extraction after step (2) being dried in step (3),
Extracting solution vibrates 24 minutes, at 4 DEG C, under the conditions of 7200 revs/min centrifugal 7 minutes, takes supernatant.
Preferably, it is characterised in that step (4) uses the supernatant in high performance liquid chromatography detecting step (3), flowing
Being ammonium formate and the formic acid 4:3 by volume mixing of 0.3% of 4.2mol/L mutually, flow velocity is 0.7mL/min, and column temperature is 26 DEG C,
Sample temperature is 5 DEG C, and sampling volume is 6 μ L.
Beneficial effect: (1) detection method of the present invention eliminates other toxin by alkaline cleaning procedure and detects 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone
Interference, improve its accuracy in detection；(2) detection method testing process of the present invention is simple, the shortest, detects into
This is relatively low.
Detailed description of the invention
Embodiment 1
In a kind of prepared slices of Chinese crude drugs, the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone, comprises the steps of
(1) adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.2kW/h, rotating speed is 2500 revs/min, put into drink per hour
Sheet amount is 2kg, attrition grinding to powdery, and powder diameter is 200 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 0.5% infiltration 0.5 hour, uses distilled water
Rinse to neutral, be placed in baking oven under the conditions of 58 DEG C drying；
(3) by step (2) dry after powder mass concentration 34% methanol extraction, extracting solution vibrate 13 minutes, 4 DEG C,
It is centrifuged 5 minutes under the conditions of 6000 revs/min, takes supernatant；
(4) using the supernatant in high performance liquid chromatography detecting step (3), flowing is the ammonium formate and 0.2% of 3mol/L mutually
Formic acid 1:3 by volume mixing, flow velocity is 0.3mL/min, and column temperature is 25 DEG C, and sample temperature is 4 DEG C, and sampling volume is 5 μ L.
Embodiment 2
In a kind of prepared slices of Chinese crude drugs, the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone, comprises the steps of
(1) adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.6kW/h, rotating speed is 2900 revs/min, put into drink per hour
Sheet amount is 4kg, attrition grinding to powdery, and powder diameter is 350 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 1.8% infiltration 2.4 hours, uses distilled water
Rinse to neutral, be placed in baking oven under the conditions of 66 DEG C drying；
(3) by step (2) dry after powder mass concentration 46% methanol extraction, extracting solution vibrate 24 minutes, 4 DEG C,
It is centrifuged 7 minutes under the conditions of 7200 revs/min, takes supernatant；
(4) using the supernatant in high performance liquid chromatography detecting step (3), flowing is the ammonium formate and 0.3% of 4.2mol/L mutually
Formic acid 4:3 by volume mixing, flow velocity is 0.7mL/min, and column temperature is 26 DEG C, and sample temperature is 5 DEG C, and sampling volume is 6 μ L.
Embodiment 3
In a kind of prepared slices of Chinese crude drugs, the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone, comprises the steps of
(1) adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.8kW/h, rotating speed is 3200 revs/min, put into drink per hour
Sheet amount is 5kg, attrition grinding to powdery, and powder diameter is 400 mesh；
(2) powder that step (1) obtains is placed in the sodium carbonate that mass concentration is 2.5% infiltration 3 hours, rushes with distilled water
It is washed till neutrality, is placed in baking oven under the conditions of 75 DEG C drying；
(3) by step (2) dry after powder mass concentration 56% methanol extraction, extracting solution vibrate 28 minutes, 4 DEG C,
It is centrifuged 10 minutes under the conditions of 8000 revs/min, takes supernatant；
(4) using the supernatant in high performance liquid chromatography detecting step (3), flowing is the ammonium formate and 0.4% of 5mol/L mutually
Formic acid 5:3 by volume mixing, flow velocity is 0.8mL/min, and column temperature is 28 DEG C, and sample temperature is 8 DEG C, and sampling volume is
10μL。
Using the detection method described in above-described embodiment 1～3 to detect the 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in the prepared slices of Chinese crude drugs, result is as follows
Shown in table:
Claims (5)
1. the detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in prepared slices of Chinese crude drugs, it is characterised in that comprise the steps of
(1) adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.2～1.8kW/h, rotating speed is 2500～3200 revs/min, every
Hour input decoction pieces amount is 2～5kg, 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% infiltration 0.5～3 hour,
With distilled water flushing to neutral, it is placed in baking oven under the conditions of 58～75 DEG C drying；
(3) powder mass concentration 34～56% methanol extraction after step (2) being dried, extracting solution vibrates 13～28 minutes,
At 4 DEG C, under the conditions of 6000～8000 revs/min centrifugal 5～10 minutes, take supernatant；
(4) use the supernatant in high performance liquid chromatography detecting step (3), flowing be mutually 3～5mol/L ammonium formate and 0.2～
The formic acid of 0.4% by volume 1～5:3 mixing, flow velocity is 0.3～0.8mL/min, and column temperature is 25～28 DEG C, sample temperature be 4～
8 DEG C, sampling volume is 5～10 μ L.
The detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs the most according to claim 1, it is characterised in that step (1)
Middle adding in pulverizer by the prepared slices of Chinese crude drugs, power is 1.6kW/h, rotating speed is 2900 revs/min, put into decoction pieces amount per hour
For 4kg, attrition grinding to powdery, powder diameter is 350 mesh.
The detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs the most according to claim 1, it is characterised in that step (2)
Middle being placed in the sodium carbonate that mass concentration is 1.8% by the powder that step (1) obtains infiltrates 2.4 hours, uses distilled water flushing
To neutral, it is placed in baking oven under the conditions of 66 DEG C drying.
The detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs the most according to claim 1, it is characterised in that step (3)
Middle by step (2) dry after powder mass concentration 46% methanol extraction, extracting solution vibrate 24 minutes, 4 DEG C, 7200
It is centrifuged 7 minutes under the conditions of rev/min, takes supernatant.
The detection method of 6-(10-hydroxy-6-oxo-trans-1-undecenyl)-.beta.-resorcylic acid lactone in a kind of prepared slices of Chinese crude drugs the most according to claim 1, it is characterised in that step (4)
Supernatant in middle employing high performance liquid chromatography detecting step (3), flowing is ammonium formate and the first of 0.3% of 4.2mol/L mutually
Acid 4:3 by volume mixes, and flow velocity is 0.7mL/min, and column temperature is 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 |
-
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 |
|---|
| 毛丹 等: "中药中玉米赤霉烯酮的残留测定", 《齐鲁药事》 * |
| 申红红 等: "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", 《中华中医药杂志》 * |
| 谭婧 等: "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", 《时珍国医国药》 * |
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