CN207938573U - A kind of on-line extraction purification needle point electrospray ionization device - Google Patents

A kind of on-line extraction purification needle point electrospray ionization device Download PDF

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Publication number
CN207938573U
CN207938573U CN201820398601.6U CN201820398601U CN207938573U CN 207938573 U CN207938573 U CN 207938573U CN 201820398601 U CN201820398601 U CN 201820398601U CN 207938573 U CN207938573 U CN 207938573U
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China
Prior art keywords
syringe
needle
electrospray ionization
ionization device
line extraction
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CN201820398601.6U
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马强
吕悦广
白桦
王春
陈萌
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Chinese Academy of Inspection and Quarantine CAIQ
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Chinese Academy of Inspection and Quarantine CAIQ
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Abstract

The utility model discloses a kind of on-line extractions to purify needle point electrospray ionization device, including disposable syringe (1), syringe-driven filter (2) and metal needle (4) there are two being sequentially connected in the front end of the disposable syringe (1), junction between two syringe-driven filters (2) is provided with Graphon filler (3), the metal needle (4) is connected with high voltage power supply, it is being provided with mass spectrograph at the metal needle (4), the disposable syringe (1) is connected with peristaltic pump.Apparatus structure described in the utility model is simple, easy to operate, and using effect is good.

Description

A kind of on-line extraction purification needle point electrospray ionization device
Technical field
The utility model is related to examine detection field, more particularly to a kind of purification needle point electrospray ionization makeup of on-line extraction It sets.
Background technology
Analytical technique of mass spectrum has the characteristics that analyze speed is fast, specificity is strong and high sensitivity, is examined all the time in analysis Survey field receives favor.Ion source is mass spectrometric important component, initial mass-spectrometric technique be only capable of realizing atom, element and The analysis of isotope, the appearance of electron impact ion source makes it possible the mass spectral analyses of the small molecules such as organic compound, but needs It to operate in high vacuum conditions;Continuously improving and innovating recently as different ions technology and mass analyzer, makes Mass Spectrometer Method covers the fields such as chemistry and chemical industry, biology and life science, medicine, pharmacy, material science, environmental protection, As a kind of strong detection means.The successful research and development of the Soft ionization techniques such as electro-spray ionization, realize large biological molecule Mass spectral analysis and in atmospheric conditions implement ionization, but its design still be closed ion source structure.
The novel open type ionization techniques of ionization can be realized without complex sample pre-treatment, under atmospheric pressure environment The research direction developed the forward position as mass spectrometry art and be concerned has developed paper spraying, toothpick is sprayed, " slug flow " is received Rise direct samples, enrichment, the technology of ionization and the corresponding devices such as extraction spraying.In directly dividing for complex matrices sample Analysis, the quick analysis of the in-situ study of biological organization sample, body surface etc. achieve important breakthrough, greatly push Development of the mass-spectrometric technique in terms of real-time, surface, original position, high throughput analysis, and quickly analysis in situ is made to become mass-spectrometric technique One of important application research direction.
Utility model content
The technical problem to be solved by the present invention is to provide a kind of on-line extractions to purify needle point electrospray ionization device, adopts Carried out with described device sample detection method have the advantages that it is convenient, fast, efficient.
A kind of on-line extraction purification needle point electrospray ionization device, including disposable syringe, in the disposable injection The front end of device is sequentially connected there are two syringe-driven filter and metal needle, the connection between two syringe-driven filters Place is provided with Graphon filler, and the metal needle is connected with high voltage power supply, is provided at the metal needle Mass spectrograph, the disposable syringe are connected with peristaltic pump.
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the metal needle is N-type Customize No. 5 syringe needles of metal, a length of 50mm, outer diameter 1.07mm, internal diameter 0.69mm, wherein the internal diameter of tip portion is 0.1mm。
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the syringe-driven filter For syringe-type import membrane filter, shell uses medical grade polypropylene material, a diameter of 13mm, the syringe-driven filter Built-in filter sizes are 0.45 μm.
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the Graphon is filled out The filling amount of material is 10mg, and the Graphon filler is 120~400 mesh.
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the disposable syringe Capacity be 5mL.
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the metal needle and institute Mass spectrometric entrance is stated coaxially and at a distance of 1cm.
On-line extraction described in the utility model purifies needle point electrospray ionization device, wherein the disposable syringe, The interface of the syringe-driven filter and the metal needle is standard luer fittings.
The utility model on-line extraction purification needle point electrospray ionization device difference from prior art is:
The utility model on-line extraction purifies needle point electrospray ionization device by disposable syringe, two needle-based filterings Device, metal needle are combined, and in disposable syringe syringe, may be implemented to the simple liquid-liquid extraction of sample, compacted Under dynamic thrust of pump effect, extraction turbid flows through first syringe-driven filter, sample residue can be filtered out, in two needle-baseds Filter junction is packed with Graphon as purification filler, the matrix such as pigment that can be effectively in sorption extraction liquid, Metal needle tip application ± 4.5kV high voltages, on-line extraction purify needle point spraying and determinand are ionized progress Mass Spectrometer Method. Had the advantages that using the method that the device of the utility model is detected convenient, fast, efficient, combined type portable mass spectrograph is suitable Quick detection for sample.
The on-line extraction of the utility model purification needle point electrospray ionization device is described further below in conjunction with the accompanying drawings.
Description of the drawings
Fig. 1 is the structural schematic diagram that the utility model on-line extraction purifies needle point electrospray ionization device.
Specific implementation mode
As shown in Figure 1, a kind of on-line extraction purifies needle point electrospray ionization device, including disposable syringe 1, primary Property syringe 1 front end be sequentially connected there are two syringe-driven filter 2 and metal needle 4, between two syringe-driven filters 2 Junction be provided with Graphon filler 3, metal needle 4 is connected with high voltage power supply, is provided at metal needle 4 Mass spectrograph, disposable syringe 1 are connected with peristaltic pump.
Metal needle 4 be N-type customize No. 5 syringe needles of metal, a length of 50mm, outer diameter 1.07mm, internal diameter 0.69mm, In, the internal diameter of tip portion is 0.1mm;Syringe-driven filter 2 is syringe-type import membrane filter, and shell is poly- using medical grade The built-in filter sizes of propylene material, a diameter of 13mm, syringe-driven filter 2 are 0.45 μm.The filling of Graphon filler 3 Amount is 10mg, and Graphon filler 3 is 120~400 mesh, and the capacity of disposable syringe 1 is 5mL, metal needle 4 and mass spectrum The entrance of instrument is coaxial and at a distance of 1cm.The interface of disposable syringe 1, syringe-driven filter 2 and metal needle 4 is standard Shandong That connector.
Using the violated addition in the on-line extraction purification needle point electrospray ionization device detection cosmetics of the utility model The method of object, includes the following steps:
Accurately weigh 1.0g samples, i.e., in the positive to the syringe of disposable syringe 1 of 500 μ g/kg of spiked levels, 2mL acetonitriles are added as extractant, the disposable syringe 1 is shaken manually and carries out liquid-liquid extraction for several times, in two needles Graphon 3 is clogged as purification filler in 2 junction of hair style filter, and by standard luer fittings respectively with it is described primary Property syringe 1 be connected with metal needle 4, the disposable syringe 1 is folded up on peristaltic pump, assembling form the online extraction Take purification needle point electrospray ionization device;The wriggling flow rate pump is set as 3.5 μ L/min, apply at needle point electron spray voltage be ± 4.5kV carries out Mass Spectrometer Method using mass spectrograph;
The Illegal addition includes bifonazole, Ornidazole and clotrimazole.
The mass spectrograph is the small-sized mass spectrometry systems of Mini β, and adjusting mass spectrometer system parameter is as shown in table 1, for level-one Complete to sweep pattern, method parameter is system default parameter, and the setting of second order ms method design parameter is shown in Table 2.
The small-sized mass spectrometry system adjustment parameter tables of 1 Mini β of table
The small-sized mass spectrometry system method parameters of Illegal addition matter Mini β in 2 cosmetics of table
Embodiment described above is only that preferred embodiments of the present invention are described, not to this practicality Novel range is defined, and under the premise of not departing from the spirit of the design of the utility model, those of ordinary skill in the art are to this The various modifications and improvement that the technical solution of utility model is made should all fall into the protection of the utility model claims book determination In range.

Claims (7)

1. a kind of on-line extraction purifies needle point electrospray ionization device, it is characterised in that:Including disposable syringe (1), in institute The front end for stating disposable syringe (1) is sequentially connected there are two syringe-driven filter (2) and metal needle (4), described in two Junction between syringe-driven filter (2) is provided with Graphon filler (3), the metal needle (4) and high voltage power supply It is connected, is being provided with mass spectrograph at the metal needle (4), the disposable syringe (1) is connected with peristaltic pump.
2. on-line extraction according to claim 1 purifies needle point electrospray ionization device, it is characterised in that:The metal needle Head (4) is that N-type customizes No. 5 syringe needles of metal, a length of 50mm, outer diameter 1.07mm, internal diameter 0.69mm, wherein tip portion Internal diameter is 0.1mm.
3. on-line extraction according to claim 2 purifies needle point electrospray ionization device, it is characterised in that:The needle-based Filter (2) is syringe-type import membrane filter, and shell uses medical grade polypropylene material, a diameter of 13mm, the syringe needle The built-in filter sizes of formula filter (2) are 0.45 μm.
4. on-line extraction according to claim 3 purifies needle point electrospray ionization device, it is characterised in that:The graphitization The filling amount of carbon black filler (3) is 10mg, and the Graphon filler (3) is 120~400 mesh.
5. on-line extraction according to claim 4 purifies needle point electrospray ionization device, it is characterised in that:It is described disposable The capacity of syringe (1) is 5mL.
6. on-line extraction according to claim 5 purifies needle point electrospray ionization device, it is characterised in that:The metal needle Head (4) is coaxial with the mass spectrometric entrance and at a distance of 1cm.
7. on-line extraction according to claim 6 purifies needle point electrospray ionization device, it is characterised in that:It is described disposable The interface of syringe (1), the syringe-driven filter (2) and the metal needle (4) is standard luer fittings.
CN201820398601.6U 2018-03-23 2018-03-23 A kind of on-line extraction purification needle point electrospray ionization device Active CN207938573U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110646498A (en) * 2019-07-08 2020-01-03 中国检验检疫科学研究院 Method for rapidly detecting rhodamine B in hotpot condiment and forchlorfenuron in watermelon

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110646498A (en) * 2019-07-08 2020-01-03 中国检验检疫科学研究院 Method for rapidly detecting rhodamine B in hotpot condiment and forchlorfenuron in watermelon

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