CN203732332U - Benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials - Google Patents
Benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials Download PDFInfo
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- CN203732332U CN203732332U CN201420040528.7U CN201420040528U CN203732332U CN 203732332 U CN203732332 U CN 203732332U CN 201420040528 U CN201420040528 U CN 201420040528U CN 203732332 U CN203732332 U CN 203732332U
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- centrifuge tube
- benzo
- disposable needle
- pyrene
- crude drug
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Abstract
The utility model discloses a benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials. The kit comprises a kit body, wherein an extracting agent centrifugal tube, a disperse co-extraction solvent centrifugal tube, an eluting agent centrifugal tube and two disposable needle tube type filters are arranged in the kit body; the extracting agent centrifugal tube and the eluting agent centrifugal tube are screw cap polypropylene conical bottom centrifugal tubes with stoppers; the disperse co-extraction solvent centrifugal tube is a screw cap polypropylene flat-bottom centrifugal tube with a stopper; the first disposable needle tube type filter consists of a cylindrical plug, a polypropylene cylinder and a needle plug; an upper sieve baffle, double-layer packing and a lower sieve baffle are arranged in the polypropylene cylinder from top to bottom; the second disposable needle tube type filter consists of a cylindrical piston, a polypropylene cylinder and a needle head type filter; a filter membrane is arranged in the needle head type filter. The kit has the advantages of reasonable structure, low manufacturing cost, simple operation, slight environmental pollution, high stability, high interference resistance and the like and is convenient to popularize, and the requirements for reducing the solvent use amount and improving the extraction efficiency can be met.
Description
Technical field
The utility model relates to food security technical field, particularly relates to benzo in a kind of Chinese crude drug (a) pyrene and detects pretreatment reagent kit.
Background technology
Benzo (a) pyrene (Benzo (a) Pyrene, B (a) P) be one of representative in polycyclic aromatic hydrocarbons, internationally recognized strong carcinogen, all can be absorbed by human body or animal by respiratory tract, alimentary canal, skin etc., can cause tumour and the canceration of humans and animals, when high dose, even can cause immunosupress, health is caused to potential threat.Under normal temperature, be light yellow crystalline solid, molecular formula is C20H12, relative molecular mass is 252, boiling point 310-320 DEG C, fusing point 179-180 DEG C, is soluble in the organic solvents such as cyclohexane, hexane, benzene, is slightly soluble in ethanol, methyl alcohol, when benzo (a) pyrene is used 360nm UV-irradiation, can produce typical purple fluorescence.
In Chinese crude drug, it is residual is mainly owing in process, raw material being toasted, steam stir-fry repeatedly, causes burning phenomenon and temperature control is improper, generates benzo (a) pyrene, remains on the shell of raw material.In recent years, China, European Union and Korea S etc. are multinational has strict limit standard to benzo in food (a) pyrene content: Chinese medicine and grain are generally no more than 5 μ g/kg.China GB2762-2005 " food contaminant limitation " regulation limitation is 10 μ g/kg.Therefore carry out the detection technique research of benzo (a) pyrene residual quantity, the risk assessment of Chinese crude drug being carried out to science is very important with monitoring.
The difficult point that benzo (a) pyrene detects is effectively to get rid of and disturb, interference comprise use reagent bring into sample substrate in intrinsic two parts, agent treated is that benzo (a) pyrene detects the false-positive key step of eliminating, in some reagent, once found that benzo (a) pyrene content even exceeded the phenomenon of food standard limitation, the result of sample pre-treatments will directly affect accuracy and the reliability of testing result simultaneously.
Sample pre-treatments mainly comprises to be extracted and purifies.In the mensuration about benzo (a) pyrene of having reported, mostly adopt traditional ultrasonic assisted extraction, and object in liquid-liquid extraction method and solid phase extraction extraction sample.The a large amount of poisonous and hazardous organic reagents of this method consumption, loaded down with trivial details time-consuming, in extraction process, easily produce a large amount of emulsifying agents, affect extraction efficiency, and need professional extraction equipment, cost high, be difficult to promote at common small-size laboratory, its range of application is restricted.
In addition, the detection pre-treating method of the standard such as existing GB GB/T5009.27-2003 " mensuration of benzo in food (a) pyrene ", GB/T22509-2008 " the mensuration reversed-phased high performace liquid chromatographic of animal and plant fat benzo (a) pyrene " and industry standard NY/T919-2004 " the mensuration high performance liquid chromatography of benzo in feed (a) pyrene ", NY/T1666-2008 " the mensuration high performance liquid chromatography of benzo in meat products (a) pyrene " is not all suitable for Chinese crude drug.Therefore, set up a kind of effective, actual amount is few, convenient fast and extremely urgent for the pretreating device of this matrix of Chinese crude drug.
Utility model content
Technical problem to be solved in the utility model is, provides a kind of extraction efficiency high and can effectively go benzo in deimpurity Chinese crude drug (a) pyrene to detect pretreatment reagent kit.
In order to solve the problems of the technologies described above, the technical solution adopted in the utility model is: benzo in a kind of Chinese crude drug (a) pyrene detects pretreatment reagent kit, comprise kit box body, extraction agent centrifuge tube is housed in kit box body, disperse extraction aid centrifuge tube, eluent centrifuge tube and two disposable needle tube type filtrators, extraction agent centrifuge tube and eluent centrifuge tube are tool plug screw top conical bottom centrifuge tube, disperseing extraction aid centrifuge tube is the flat centrifuge tube of tool plug screw top, first disposable needle tube type filtrator is by cylinder plug, cylinder and syringe needle plug form, gear sieve plate is from top to bottom housed in cylinder, double-deck filler, lower block sieve plate, second disposable needle tube type filtrator is made up of column piston, cylinder and syringe-driven filter, has filter membrane in syringe-driven filter, eluent in extraction agent and eluent centrifuge tube in described extraction agent centrifuge tube is the chromatographically pure cyclohexane heavily steaming through activated charcoal, disperseing the dispersion extraction aid in extraction aid centrifuge tube is the white powder potpourri of sodium chloride and anhydrous magnesium sulfate, filler in first disposable needle tube type filtrator is upper strata anhydrous sodium sulfate, lower floor's neutral alumina, and injection ring hexane soaked the surface of filler.
Described extraction agent centrifuge tube, dispersion extraction aid centrifuge tube and eluent centrifuge tube are polypropylene tube, and described first disposable needle tube type filtrator and second disposable needle tube type filtrator are polyethylene pipe.
Described extraction agent centrifuge tube and eluent centrifuge tube capacity are respectively 20-50mL.
The capacity of described dispersion extraction aid centrifuge tube is 15-20mL.
The cylinder capacity of described first disposable needle tube type filtrator is 50-70mL, and the cylinder capacity of second disposable needle tube type filtrator is 10-30mL.
The screen size of described upper gear sieve plate and lower block sieve plate is 0.15-0.30 μ m.
In described syringe filters, there is the filter membrane of 0.3-0.8 μ m.
Cyclohexane liquid level in described first disposable needle tube type filtrator is higher than upper gear sieve plate 5mm.
The beneficial effects of the utility model are:
(1) simple, pollution-free, the room temperature preservation of manufacturing process;
(2) pretreatment process only needed about 20 minutes, fast simple, and single part of mensuration is spent low;
(3) extraction agent is cyclohexane solution, has reduced the polarity of extracting solvent, and benzo in Chinese crude drug (a) pyrene is had to high selectivity extractability, has reduced the liquid water content in moisture class matrix extract, has alleviated the follow-up water pressure of removing;
(4) disperse anhydrous magnesium sulfate heat production in water suction in extraction aid, promoted the extraction of target compound; ,
(5) in disposable needle tube type filtrator, filler has effective removing ability to impurity in Chinese crude drug;
(6) this kit formation is simple, reasonable, economical and practical, is conducive to promote the use of.
Brief description of the drawings
Fig. 1 is that benzo in the utility model Chinese crude drug (a) pyrene detects pretreatment reagent kit structural representation;
Fig. 2 is that in the Chinese crude drug that provides with the utility model of Chinese crude drug matrix sample, benzo (a) pyrene detects pretreatment reagent kit blank spectrogram after treatment;
Fig. 3 is that benzo (a) pyrene that Chinese crude drug matrix sample provides with the utility model detects the 2.5 μ g/kg mark-on HPLC spectrograms that pretreatment reagent kit sample introduction after treatment is analyzed;
Fig. 4 is that benzo (a) pyrene that Chinese crude drug matrix sample provides with the utility model detects the 5.0 μ g/kg mark-on HPLC spectrograms that pretreatment reagent kit sample introduction after treatment is analyzed;
Fig. 5 is benzo (a) pyrene typical curve.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail:
As shown in Figure 1, benzo in Chinese crude drug of the present utility model (a) pyrene detects pretreatment reagent kit, kit box body, extraction agent centrifuge tube 1 is housed in kit box body, disperse extraction aid centrifuge tube 2, eluent centrifuge tube 3 and two disposable needle tube type filtrators, extraction agent centrifuge tube 1 and eluent centrifuge tube 3 are tool plug screw top conical bottom centrifuge tube, disperseing extraction aid centrifuge tube 2 is the flat centrifuge tube of tool plug screw top, first disposable needle tube type filtrator 4 is by cylinder plug, cylinder and syringe needle plug form, gear sieve plate is from top to bottom housed in cylinder, double-deck filler, lower block sieve plate, second disposable needle tube type filtrator 5 is made up of column piston, cylinder and syringe-driven filter, has filter membrane in syringe-driven filter, eluent in extraction agent and eluent centrifuge tube 3 in described extraction agent centrifuge tube 1 is the chromatographically pure cyclohexane heavily steaming through activated charcoal, disperseing the dispersion extraction aid in extraction aid centrifuge tube 2 is the white powder potpourri of sodium chloride and anhydrous magnesium sulfate, filler in first disposable needle tube type filtrator 4 is upper strata anhydrous sodium sulfate, lower floor's neutral alumina, and injection ring hexane soaked the surface of filler.
Described extraction agent centrifuge tube 1, dispersion extraction aid centrifuge tube 2 and eluent centrifuge tube 3 are polypropylene tube, and described first disposable needle tube type filtrator 4 and second disposable needle tube type filtrator 5 are polyethylene pipe.
Described extraction agent centrifuge tube 1 and eluent centrifuge tube 3 capacity are respectively 20-50mL.
The capacity of described dispersion extraction aid centrifuge tube 2 is 15-20mL.
The cylinder capacity of described first disposable needle tube type filtrator 4 is 50-70mL, and the cylinder capacity of second disposable needle tube type filtrator 5 is 10-30mL.
The screen size of described upper gear sieve plate and lower block sieve plate is 0.15-0.30 μ m.
In described syringe filters, there is the filter membrane of 0.3-0.8 μ m.
Cyclohexane liquid level in described first disposable needle tube type filtrator 4 is higher than upper gear sieve plate 5mm.
For further understanding technology contents of the present utility model, features and action, hereby exemplify following examples, and coordinate accompanying drawing to be described in detail as follows:
Benzo in Chinese crude drug (a) pyrene detects pretreatment reagent kit, comprises extraction agent centrifuge tube 1, disperses extraction aid centrifuge tube 2, eluent centrifuge tube 3, fills Packed first disposable needle tube type filtrator 4, second disposable needle tube type filtrator 5 containing filter membrane.
Preferably, extraction agent and eluent are contained in 50mL tool plug screw top polypropylene conical bottom centrifuge tube, disperse extraction aid to be contained in the flat centrifuge tube of 20mL tool plug screw top polypropylene.
Preferably, extraction agent is chromatographically pure chemistry reagent, the cyclohexane heavily steaming through activated charcoal.Cyclohexane occurred mixing in a large number on chromatogram peak and have a small amount of benzo (a) pyrene, therefore utilize benzo (a) pyrene can be by positively charged adsorbent---the characteristic of charcoal absorption, after adding activated charcoal redistillation in cyclohexane, re-use, test findings shows that effect is fine.
Preferably, disperseing extraction aid is the white powder potpourri of sodium chloride and anhydrous magnesium sulfate.
Preferably, the cylinder capacity of first disposable needle tube type filtrator 4 is 70mL.
Further, first disposable needle tube type filtrator 4 is made up of tygon cylinder plug, transparent polyethylene cylinder and tygon syringe needle plug, and gear sieve plate, double-deck filler, 0.22 μ m lower block sieve plate on 0.22 μ m are from top to bottom housed in tygon cylinder.
Further, double-deck filler upper strata is sodium chloride, lower floor is IV level neutral alumina powder, and its activity determination method is with reference to appendix A in standard GB/T/T22509-2008 " the mensuration reversed-phased high performace liquid chromatographic of animal and plant fat benzo (a) pyrene ".
Preferably, the cylinder capacity of second disposable needle tube type filtrator 5 is 10mL.
Further, in syringe filters, there is the filter membrane of 0.45 μ m.
The preparation of described kit:
The preparation of described extraction agent: the cyclohexane solution 25mL that preparation is heavily steamed through activated charcoal, is transferred in 50mL tool plug screw top polypropylene conical bottom centrifuge tube.
The preparation of described dispersion extraction aid: take 2g sodium chloride and 2g anhydrous magnesium sulfate fully mixes, be transferred in the flat centrifuge tube of 20mL tool plug screw top polypropylene.
The preparation of described eluent: the cyclohexane solution 50mL that preparation is heavily steamed through activated charcoal, is transferred in 50mL tool plug screw top polypropylene conical bottom centrifuge tube.
First described disposable needle tube type filtrator preparation: in disposable needle tube type filtrator, purification filler is housed, it is double-deck purifying filler, and upper strata is 5g sodium chloride, and lower floor is 30g IV level neutral alumina powder.
First described disposable needle tube type filtrator loaded process: cylinder bottom pad last layer 0.22 μ m lower block sieve plate now, add lower floor's filler and upper strata filler, cover on one deck 0.22 μ m again and keep off sieve plate on filler top, put into cyclohexane, liquid level is higher than upper gear sieve plate 5mm left and right.
Second described disposable needle tube type filtrator can be measured as liquid chromatograph entering analytical instrument after traditional Chinese medicinal material samples solution filter.
Concrete application implementation of the present utility model:
1, get benzo in Chinese crude drug (a) pyrene and detect pretreatment reagent kit, comprise extraction agent centrifuge tube, disperse extraction aid centrifuge tube, eluent centrifuge tube and two disposable needle tube type filtrators.
2, the Chinese crude drug containing benzo (a) pyrene pulverized to sample and disperseed extraction aid to put into extraction agent centrifuge tube and mix, shake well obtains mixed solution, the centrifugal 3min of 14000r/min.Take off cylinder plug and the column cap plug of first disposable needle tube type filtrator, by supernatant, through first disposable needle tube type filtrator, leacheate also oozes to conical flask naturally through first disposable needle tube type filtrator.To mix filtrate rotary evaporated to dryness in 45 DEG C of water-baths, accurately add 1mL acetonitrile and dissolve constant volume, after fully mixing, after filtering, second disposable needle tube type filtrator deposit in sample injection bottle, measure for liquid chromatograph, result extraction recovery reaches 75.2%-109.1%, meets mensuration requirement.
3, with in blank Chinese crude drug matrix sample, add benzo (a) the pyrene standard solution of 2.5 μ g/kg and 5.0 μ g/kg, with 2 operations, sample solution injection liquid chromatography is measured.
The results are shown in Figure 2 to Fig. 5, Fig. 2 is that in the Chinese crude drug that provides with the utility model of Chinese crude drug matrix sample, benzo (a) pyrene detects pretreatment reagent kit blank spectrogram after treatment, Fig. 3 is that benzo (a) pyrene that Chinese crude drug matrix sample provides with the utility model detects the 2.5 μ g/kg mark-on HPLC spectrograms that pretreatment reagent kit sample introduction after treatment is analyzed, Fig. 4 is that benzo (a) pyrene that Chinese crude drug matrix sample provides with the utility model detects the 5.0 μ g/kg mark-on HPLC spectrograms that pretreatment reagent kit sample introduction after treatment is analyzed, Fig. 5 is benzo (a) pyrene typical curve.
The utility model extraction efficiency is high and can effectively remove impurity, for quick pretreatment Chinese crude drug benzo (a) pyrene, can directly carry out liquid chromatograph detection through this kit sample after treatment.Benzo in Chinese crude drug (a) pyrene detects pretreatment reagent kit to be had and the advantage such as forms rationally, cost of manufacture is low, simple to operate, environmental pollution is little, good stability, antijamming capability are strong, and can meet the demand that reduces solvent use amount and improve extraction efficiency, be convenient to promote.And the instrumental analysis pre-treating method of measuring for further integrating and finally set up benzo (a) pyrene of system, reference and data accumulation are provided.
Above-described embodiment is only for illustrating technological thought of the present utility model and feature, its object is to make those skilled in the art can understand content of the present utility model and implement according to this, can not only limit the scope of the claims of the present utility model with the present embodiment, be equal variation or the modification that spirit that all the utility model disclose is done, still drop in the scope of the claims of the present utility model.
Claims (8)
1. in a Chinese crude drug, benzo (a) pyrene detects pretreatment reagent kit, comprise kit box body, it is characterized in that, extraction agent centrifuge tube (1) is housed in kit box body, disperse extraction aid centrifuge tube (2), eluent centrifuge tube (3) and two disposable needle tube type filtrators, extraction agent centrifuge tube (1) and eluent centrifuge tube (3) are tool plug screw top conical bottom centrifuge tube, disperseing extraction aid centrifuge tube (2) is the flat centrifuge tube of tool plug screw top, first disposable needle tube type filtrator (4) is by cylinder plug, cylinder and syringe needle plug form, gear sieve plate is from top to bottom housed in cylinder, double-deck filler, lower block sieve plate, second disposable needle tube type filtrator (5) is made up of column piston, cylinder and syringe-driven filter, has filter membrane in syringe-driven filter, eluent in extraction agent in described extraction agent centrifuge tube (1) and eluent centrifuge tube (3) is the chromatographically pure cyclohexane heavily steaming through activated charcoal, disperseing the dispersion extraction aid in extraction aid centrifuge tube (2) is the white powder potpourri of sodium chloride and anhydrous magnesium sulfate, filler in first disposable needle tube type filtrator (4) is upper strata anhydrous sodium sulfate, lower floor's neutral alumina, and injection ring hexane soaked the surface of filler.
2. in Chinese crude drug according to claim 1, benzo (a) pyrene detects pretreatment reagent kit, it is characterized in that, described extraction agent centrifuge tube (1), dispersion extraction aid centrifuge tube (2) and eluent centrifuge tube (3) are polypropylene tube, and described first disposable needle tube type filtrator (4) and second disposable needle tube type filtrator (5) are polyethylene pipe.
3. in Chinese crude drug according to claim 1, benzo (a) pyrene detects pretreatment reagent kit, it is characterized in that, described extraction agent centrifuge tube (1) and eluent centrifuge tube (3) capacity are respectively 20-50mL.
4. in Chinese crude drug according to claim 3, benzo (a) pyrene detects pretreatment reagent kit, it is characterized in that, the capacity of described dispersion extraction aid centrifuge tube (2) is 15-20mL.
5. in Chinese crude drug according to claim 4, benzo (a) pyrene detects pretreatment reagent kit, it is characterized in that, the cylinder capacity of described first disposable needle tube type filtrator (4) is 50-70mL, and the cylinder capacity of second disposable needle tube type filtrator (5) is 10-30mL.
6. benzo (a) pyrene detects pretreatment reagent kit in Chinese crude drug according to claim 1 or 5, it is characterized in that, the screen size of described upper gear sieve plate and lower block sieve plate is 0.15-0.30 μ m.
7. benzo (a) pyrene detects pretreatment reagent kit in Chinese crude drug according to claim 1 or 5, it is characterized in that in described disposable needle tube type filtrator, there is the filter membrane of 0.3-0.8 μ m.
8. in Chinese crude drug according to claim 1, benzo (a) pyrene detects pretreatment reagent kit, it is characterized in that, the cyclohexane liquid level in described first disposable needle tube type filtrator (4) is higher than upper gear sieve plate 5mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420040528.7U CN203732332U (en) | 2014-01-22 | 2014-01-22 | Benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420040528.7U CN203732332U (en) | 2014-01-22 | 2014-01-22 | Benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials |
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| CN201420040528.7U Expired - Fee Related CN203732332U (en) | 2014-01-22 | 2014-01-22 | Benzo(a)pyrene detection pretreatment kit in traditional Chinese medicinal materials |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316484A (en) * | 2014-11-13 | 2015-01-28 | 中国日用化学工业研究院 | Method for detecting benzo (a) pyrene in medium and high-temperature coal pitch |
| CN106124645A (en) * | 2016-06-12 | 2016-11-16 | 浙江工商大学 | Needle-based Solid-Phase Extraction filter |
| WO2020191528A1 (en) * | 2019-03-22 | 2020-10-01 | 巨研科技股份有限公司 | Kit for extracting drug residues from livestock, poultry and aquatic products, and method for obtaining primary test liquid |
-
2014
- 2014-01-22 CN CN201420040528.7U patent/CN203732332U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104316484A (en) * | 2014-11-13 | 2015-01-28 | 中国日用化学工业研究院 | Method for detecting benzo (a) pyrene in medium and high-temperature coal pitch |
| CN104316484B (en) * | 2014-11-13 | 2017-03-29 | 中国日用化学工业研究院 | Benzo in a kind of medium and high temperature coal tar pitch（a）The detection method of pyrene |
| CN106124645A (en) * | 2016-06-12 | 2016-11-16 | 浙江工商大学 | Needle-based Solid-Phase Extraction filter |
| WO2020191528A1 (en) * | 2019-03-22 | 2020-10-01 | 巨研科技股份有限公司 | Kit for extracting drug residues from livestock, poultry and aquatic products, and method for obtaining primary test liquid |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140723 Termination date: 20150122 |
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| EXPY | Termination of patent right or utility model |