CN208060458U - The in-line purification and solid-phase extraction device of carbendazim in a kind of measurement orange juice - Google Patents
The in-line purification and solid-phase extraction device of carbendazim in a kind of measurement orange juice Download PDFInfo
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Abstract
A kind of in-line purification and solid-phase extraction device measuring carbendazim in orange juice disclosed by the utility model, including enrichment pump, analysis pump, autosampler, ten-way valve, column oven, SPE columns, analytical column and diode array detector；The analysis pump is with enrichment pump group at double pump, wherein enrichment pump discharge connects autosampler input terminal, analytical column is set in column oven.The utility model is not only not necessarily to cumbersome manual operation, but also has the characteristics that high sensitivity, at low cost, environmental-friendly.
Description
Technical field
The utility model belong to chromatography detection and field of food detection, more particularly to it is a kind of measure orange juice in carbendazim
Line purifies and solid-phase extraction device.
Background technology
As a kind of wide-spectrum bactericide, carbendazim is widely used in the prevention and control of plant diseases, pest control of the fruit trees such as orange, it is therefore possible to
Lead to the residual of carbendazim in the fruit drinks such as orange juice.Due to the carbendazim longevity of residure is longer and in the world to carbendazim in orange juice
Have and clearly limit the quantity, therefore it is very necessary to carry out effective measure to the content of carbendazim in orange juice.High performance liquid chromatography
It is the common method for measuring carbendazim in orange juice.Due to the complicated component of orange juice, sample pre-treatments are to measure carbendazim in orange juice
The important step of content.The method reported at present mostly uses the mode of offline solid phase extraction column extraction, purification, such as SN/T
1753-2006 <<Import and export probenazole, Determination of carbendazim residue detection method high performance liquid chromatography in inspissated juice>>, mistake
Journey is complicated, cumbersome, and solid phase extraction column can not be reused, cost is higher.
In view of this, the present inventor combines in-line purification/Solid Phase Extraction and high performance liquid chromatography, a kind of measurement is provided
Purification/SPE HPLC of carbendazim, under conditions of handling before avoiding complex sample and is at low cost, to orange
Carbendazim in juice is effectively measured.
Utility model content
The purpose of this utility model is to provide it is a kind of measurement orange juice in carbendazim in-line purification and solid-phase extraction device,
It is not only not necessarily to cumbersome manual operation, but also has the characteristics that high sensitivity, at low cost, environmental-friendly.
To achieve the goals above, the technical solution of the utility model is as follows：
The in-line purification and solid-phase extraction device of carbendazim in a kind of measurement orange juice, including enrichment pump, analysis pump, automatically into
Sample device, ten-way valve, column oven, SPE columns, analytical column and diode array detector；Analysis pump and enrichment pump group at double pump,
Wherein enrichment pump discharge connects autosampler input terminal, and analytical column is set in column oven；
Purify/Solid Phase Extraction when, the autosampler output end was connected ten-way valve and was connect and SPE column input terminals
It is connected, SPE column output ends connect waste water by ten-way valve；The analysis pump discharge connects analytical column input terminal by ten-way valve, point
Analyse column output termination diode array detector input terminal；
When carrying out chromatography, the autosampler output end was connected ten-way valve and connect to be connected with SPE column input terminals
It connects, SPE columns output end connects analytical column input terminal, analytical column output termination diode array detector input terminal by ten-way valve；
The analysis pump discharge connects extraneous air by ten-way valve.
Further, purify/Solid Phase Extraction when, No. 6 positions of the autosampler output termination ten-way valve, No. 6 positions
With No. 5 position intercommunications, and No. 5 positions connect No. 8 positions, No. 8 positions and No. 7 position intercommunications, and No. 7 positions connect SPE column input terminals, SPE outputs termination 2
Position, No. 2 positions and No. 1 position intercommunication, No. 1 position connects waste liquid；The analysis pump discharge connects No. 4 positions of ten-way valve, No. 4 positions and No. 3 position intercommunications,
No. 3 positions connect analytical column input terminal, analytical column output termination diode detector；
When carrying out chromatography, the autosampler, which exports, terminates No. 6 positions of ten-way valve, No. 6 positions and No. 7 position intercommunications, and 7
Number position connects SPE column input terminals, No. 2 positions of SPE columns output termination, and No. 2 positions and No. 3 position intercommunications, No. 3 positions connect analytical column input terminal, point
Analysis column output connects diode detector；The analysis pump discharge connects No. 4 positions, No. 4 positions and No. 5 position intercommunications, while No. 5 positions connect No. 8
Position, No. 8 positions and No. 9 position intercommunications, No. 9 positions connect extraneous air.
After adopting the above scheme, the utility model has the beneficial effect that：The utility model passes through in-line purification/Solid Phase Extraction skill
Art is automatically performed enrichment and the purification process of sample, avoids complicated artificial pre-treatment operation, not only reduces human error, carries
High method accuracy, and it is repeatable few using solid-phase extraction column, required organic solvent；In combination with high performance liquid chromatograph sheet
Body efficiently separation and quantitation capabilities, realize under without complicated Pretreatment, easy, accurate and environmentally friendly survey
Determine carbendazim concentration in orange juice.It is also right while carbendazim residual of the utility model in order to control in beverage provides technical support
It detects pesticide in other complex matrices and remains important reference.
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail.
Description of the drawings
Fig. 1 is that the utility model measures carbendazim general flow chart in orange juice；
Fig. 2 and 3 the utility model are in in-line purification/Solid Phase Extraction and clastotype figure；
Fig. 4 is the uv absorption spectra of carbendazim standard solution；
Fig. 5 is 5 μ g/L carbendazim standard products (a) of concentration, juice samples (b) and blank sample (c) chromatogram.
Label declaration
Enrichment pump 1, analysis pump 2, autosampler 3, ten-way valve 4, SPE columns 5, analytical column 6, diode array detector 7.
Specific implementation mode
As shown in Figures 2 and 3, the in-line purification and Solid Phase Extraction of carbendazim in a kind of measurement orange juice that the utility model discloses
Device, including enrichment pump 1, analysis pump 2, autosampler 3, ten-way valve 4, column oven（It is not shown in figure）, SPE columns 5, analytical column
6 and diode array detector 7；Analysis pump 2 and 1 composition double pump of enrichment pump, wherein to connect autosampler 3 defeated for 1 outlet of enrichment pump
Enter end, analytical column 6 is also set in column oven；
Purify/Solid Phase Extraction when, 3 output end of autosampler was connected ten-way valve 4 and was connect and 5 input terminal of SPE columns
It is connected, 5 output end of SPE columns connects waste water by ten-way valve 4；2 outlet of analysis pump connects 6 input terminal of analytical column by ten-way valve, point
Analyse output termination 7 input terminal of diode array detector of column 6；
When carrying out chromatography, 3 output end of the autosampler was connected ten-way valve 4 and was connect and 5 input terminal phase of SPE columns
Connection, 5 output end of SPE columns connect analytical column input terminal by ten-way valve 4, and the output termination diode array detector 7 of analytical column 6 is defeated
Enter end；2 outlet of analysis pump connects extraneous air by ten-way valve.
Purify/Solid Phase Extraction when, No. 6 positions of the output termination ten-way valve of autosampler 3, No. 6 positions and No. 5 positions are mutual
It is logical, and No. 5 positions connect No. 8 positions, No. 8 positions and No. 7 position intercommunications, No. 7 positions connect SPE column input terminals, No. 2 positions of SPE output terminations, No. 2 positions
With No. 1 position intercommunication, No. 1 position connects waste liquid；The analysis pump discharge connects No. 4 positions of ten-way valve, No. 4 positions and No. 3 position intercommunications, and No. 3 positions connect
Analytical column input terminal, the output termination diode detector of analytical column 6；
When carrying out chromatography, the autosampler, which exports, terminates No. 6 positions of ten-way valve, No. 6 positions and No. 7 position intercommunications, and 7
Number position connects SPE column input terminals, No. 2 positions of SPE columns output termination, and No. 2 positions and No. 3 position intercommunications, No. 3 positions connect analytical column input terminal, point
Analysis column output connects diode detector；The analysis pump discharge connects No. 4 positions, No. 4 positions and No. 5 position intercommunications, while No. 5 positions connect No. 8
Position, No. 8 positions and No. 9 position intercommunications, No. 9 positions connect extraneous air.
The present embodiment disclose a kind of to measure the in-line purification of carbendazim and solid-phase extraction device in orange juice real using above-mentioned
That applies measures the in-line purification and solid phase extraction method of carbendazim in orange juice, includes the following steps：
S1. sample pre-treatments
3.0 g orange juices are weighed in 10 mL centrifuge tubes, sequentially add 3 mL containing the acetonitrile of 1% methanol, 1.2 g magnesium sulfate and
After vibrating 1 min of mixing, 10 min are centrifuged with 8000 r/min speed for 0.3 g sodium acetates；Its supernatant is taken, is filtered with 0.45 μm
Sample solution to be measured is obtained after membrane filtration；Blank sample is carried out at the same time identical sample pre-treatments with sample, obtains blank sample
Solution；
S2. the preparation of standard solution
0.1 mg carbendazim standard products are weighed in 100 mL volumetric flasks, graduation mark is settled to acetone, shakes up, obtain dense
Degree is 1 mg/L carbendazim standard reserving solutions；1 mL carbendazim storing solutions are taken, 10 mL is settled to deionized water, obtains concentration
For 100 μ g/L carbendazim standard solution；Take a concentration of 100 μ g/L carbendazim standard solution of 1 mL, 2 mL, 5 mL to three respectively
In 10 different mL volumetric flasks, with deionized water constant volume, the more of a concentration of 10 μ g/L, 20 μ g/L and 50 μ g/L are obtained successively
Bacterium spirit standard reserving solution；By a concentration of 10 μ g/L, the carbendazim standard reserving solution of 20 μ g/L and 50 μ g/L use deionized water respectively
10 times are diluted respectively, concentration is obtained and is followed successively by 1.0 μ g/L, and 2.0 μ g/L, 5.0 μ g/L carbendazim standard solution are more by 5.0 μ g/L
Bacterium spirit standard reserving solution dilutes 10 times, a concentration of 0.5 μ g/L carbendazim standard solution is obtained, to obtain following standard curve
Concentration：0.5 μ g/L, 1.0 μ g/L, 2.0 μ g/L, 5.0 μ g/L, 10 μ g/L, 20 μ g/L, 50 μ g/L, 100 μ g/L；
S3. in-line purification/Solid Phase Extraction and separation
Using above-mentioned double gradient high performance liquid-chromatography apparatus to aforementioned carbendazim standard solution, sample solution and blank
Sample solution carries out machine testing, double gradient high performance liquid-chromatography apparatus pump containing enrichment 1, analysis pump 2, autosampler 3, ten
Port valve 4, column oven, SPE columns 5, analytical column 6 and diode array detector 7, referring to Fig. 2 and 3, aforementioned three kinds of solution is in double ladders
It is as follows into line purification/Solid Phase Extraction and separation process to spend highly effective liquid phase chromatographic device：
0-2 min, ten-way valve is at 4-3, and enrichment pump completes sample introduction by autosampler, and target compound is in SPE columns
Upper enrichment and impurity removal, analysis pump is in equilibrium analysis column；
2.1-4.4 min, for ten-way valve at 4-5, SPE columns are introduced into analysis flow path, and target compound is eluted from SPE columns
Get off and flows into analytical column；
4.5-10 min, for ten-way valve at 4-3, SPE columns are brought out analysis flow path, and mobile phase returns to original state, point
Analysis post separation target compound is simultaneously back to original state；
Its chromatographic condition is as follows：
（1）Purification/solid phase extraction system：
SPE columns：Thermo Acclaim Trinity P1,3 μm of Analytical, 3.0 × 100 mm
Mobile phase： A：Water, B：Methanol mobile phase gradient：A, 0-2 min, 100%；2.1-4.5 min, 50%； 4.6–
10 min, 100%
Flow velocity： 0.7 mL/min
Sampling volume： 1000 µL；
（2）Analysis system：
Analytical column：Thermo Acclaim Polar Advantage II (PA2), 3 μm of Analytical, 3.0 ×
150 mm
Mobile phase： A：100 mM ammonium formate solutions, B：Acetonitrile
Eluent gradient：A, 0-3 min, 100%；3.1-6.5 min, 100-50%；6.6-10 min, 100%
Column temperature： 30 °C
Flow velocity：1.0 mL/min
Detection wavelength： 281 nm
The Vavle switching time：0 min, 4_3；2.0 min, 4_5；4.5 min, 4_3.
S4. qualitative and quantitative analysis
S41. qualitative analysis
When sample solution examination with computer result while meeting two following conditions, then judges residual containing carbendazim in sample
It stays：
1）, the retention time of target compound is consistent with the retention time of carbendazim standard working solution in sample solution；
2）, in sample solution the full wavelength scanner result and carbendazim standard solution of target compound full wavelength scanner knot
Fruit is consistent；
S42. quantitative analysis
Referring to Fig. 3, using the uv-absorption maximum wavelength of carbendazim standard solution as Detection wavelength, carbendazim chromatography is obtained
The relative standard deviation of figure, retention time and peak area obtained by continuous 8 continuous sample introductions of target compound is less than 2%, target
The standard curve of compound has good linear（R2≥0.99）, sample concentration in standard curve range, and work as mark-on sample
The rate of recovery of product is 70-130%, since sample pre-treatments are long without concentrating and diluting, passes through the dense of standard curve acquisition on instrument
Degree is sample concentration.As shown in figure 4,5 μ g/L carbendazim standard products (a) of comparison, juice samples (b) and blank sample (c)
Chromatogram.
The equivalent variations that all mentalities of designing according to this case are done, each fall within the protection domain of this case.
Claims (2)
1. a kind of in-line purification and solid-phase extraction device measuring carbendazim in orange juice, which is characterized in that including enrichment pump, analysis
Pump, autosampler, ten-way valve, column oven, SPE columns, analytical column and diode array detector；The analysis pump is pumped with enrichment
Double pump is formed, wherein enrichment pump discharge connects autosampler input terminal, analytical column is set in column oven；
Purify/Solid Phase Extraction when, the autosampler output end was connected ten-way valve and connect to be connected with SPE column input terminals
It connects, SPE column output ends connect waste water by ten-way valve；The analysis pump discharge connects analytical column input terminal, analytical column by ten-way valve
Output termination diode array detector input terminal；
When carrying out chromatography, the autosampler output end was connected ten-way valve and connect to be connected with SPE column input terminals,
SPE columns output end connects analytical column input terminal, analytical column output termination diode array detector input terminal by ten-way valve；It is described
Analysis pump discharge connects extraneous air by ten-way valve.
2. a kind of in-line purification and solid-phase extraction device measuring carbendazim in orange juice as described in claim 1, feature exist
In：
Purify/Solid Phase Extraction when, No. 6 positions of the autosampler output termination ten-way valve, No. 6 positions and No. 5 position intercommunications,
And No. 5 positions connect No. 8 positions, No. 8 positions and No. 7 position intercommunications, No. 7 positions connect SPE column input terminals, No. 2 positions of SPE output terminations, No. 2 positions and 1
Number position intercommunication, No. 1 position connects waste liquid；The analysis pump discharge connects No. 4 positions of ten-way valve, No. 4 positions and No. 3 position intercommunications, and No. 3 positions connect analysis
Column input terminal, analytical column output termination diode detector；
When carrying out chromatography, the autosampler output terminates No. 6 positions of ten-way valve, No. 6 positions and No. 7 position intercommunications, No. 7 positions
SPE column input terminals, No. 2 positions of SPE columns output termination, No. 2 positions and No. 3 position intercommunications are connect, No. 3 positions connect analytical column input terminal, analytical column
Output connects diode detector；The analysis pump discharge connects No. 4 positions, No. 4 positions and No. 5 position intercommunications, while No. 5 positions connect No. 8 positions, 8
Number position and No. 9 position intercommunications, No. 9 positions connect extraneous air.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108195976A (en) * | 2018-02-02 | 2018-06-22 | 厦门鉴科检测技术有限公司 | The in-line purification of carbendazim and solid phase extraction method and device in a kind of measure orange juice |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108195976A (en) * | 2018-02-02 | 2018-06-22 | 厦门鉴科检测技术有限公司 | The in-line purification of carbendazim and solid phase extraction method and device in a kind of measure orange juice |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: An on line solid phase extraction device for the determination of Carbendazim Effective date of registration: 20201112 Granted publication date: 20181106 Pledgee: Xiamen Huli District Financing Guarantee Co.,Ltd. Pledgor: XIAMEN JANKO TESTING SERVICE Co.,Ltd. Registration number: Y2020980007812 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20211126 Granted publication date: 20181106 Pledgee: Xiamen Huli District Financing Guarantee Co.,Ltd. Pledgor: XIAMEN JANKO TESTING SERVICE CO.,LTD. Registration number: Y2020980007812 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: On line purification and solid phase extraction device for determining carbendazim in orange juice Effective date of registration: 20211130 Granted publication date: 20181106 Pledgee: Xiamen Huli District Financing Guarantee Co.,Ltd. Pledgor: XIAMEN JANKO TESTING SERVICE CO.,LTD. Registration number: Y2021980013710 |