阅读说明：本技术 一种固相微萃取拭子装置及方法 (Solid phase micro-extraction swab device and method ) 是由 胡斌 伍琳 袁子程 于 2019-11-05 设计创作，主要内容包括：本发明实施例公开了一种固相微萃取拭子装置及方法,具体涉及分离分析装置与方法领域,包括固相微萃取探针、采样球,所述采样球包裹于固相微萃取探针底端外部；固相微萃取探针底端插入采样球内部用于进行样品富集,并且从采样球抽出用于进一步分析被富集的样品；固相微萃取方法具体为：用固相微萃取探针对采样球内的样品进行富集；将富集样品后的探针放入预装有试剂的毛细管中进行电喷雾离子化；样品产生离子后进入质谱检测仪一侧的进样口内,从而被检测和鉴定。本发明通过将固相微萃取探针和采样球结合,通过采样湿润溶解固体样品和采集粘性样品,解决了目前固相微萃取无法直接对固体和粘液进行富集的难题,具有广阔的市场应用前景。(The embodiment of the invention discloses a solid phase micro-extraction swab device and a method, and particularly relates to the field of separation and analysis devices and methods, wherein the device comprises a solid phase micro-extraction probe and a sampling ball, wherein the sampling ball is wrapped outside the bottom end of the solid phase micro-extraction probe; the bottom end of the solid phase micro-extraction probe is inserted into the sampling ball for sample enrichment, and is extracted from the sampling ball for further analysis of the enriched sample; the solid phase micro-extraction method comprises the following steps: enriching the sample in the sampling ball by using a solid phase microextraction probe; putting the probe enriched with the sample into a capillary tube pre-filled with a reagent for electrospray ionization; and the sample generates ions and then enters a sample inlet at one side of the mass spectrum detector so as to be detected and identified. The invention combines the solid phase micro-extraction probe and the sampling ball, and solves the problem that the solid and the mucus can not be directly enriched by the solid phase micro-extraction at present by wetting and dissolving the solid sample and collecting the viscous sample by sampling, thereby having wide market application prospect.)

1. A solid phase microextraction swab device, comprising: the device comprises a solid phase micro-extraction probe (1) and a sampling ball (2), wherein the sampling ball (2) is wrapped outside the bottom end of the solid phase micro-extraction probe (1);

the bottom end of the solid phase micro-extraction probe (1) is inserted into the sampling ball (2) for sample enrichment, and is extracted from the sampling ball (2) for further analysis of the enriched sample (3).

2. A solid phase microextraction swab device according to claim 1, wherein: the sampling ball (2) is made of a wettable, porous material.

3. A solid phase microextraction swab device according to claim 2, wherein: the wettable, porous material is in particular a fibrous material or a cotton ball.

4. A solid phase microextraction swab device according to claim 3, wherein: the sampling ball (2) is used for wetting the sample, filtering impurities and isolating the probe while collecting the sample.

5. A solid phase microextraction swab device according to claim 1, wherein: the sample (3) comprises a liquid, a viscous liquid and a solid surface soluble sample.

6. A method of solid phase microextraction using the solid phase microextraction swab device of any of claims 1-5, wherein: the method specifically comprises the following steps:

step one, sampling: enriching a sample (3) in the sampling ball (2) by using a solid phase microextraction probe (1);

step two, ionization: one end of the solid phase micro-extraction probe (1) after enriching the sample is put into a capillary tube (6) pre-filled with a reagent (4) for electrospray ionization;

step three, detection: ions (5) generated by the sample (3) enter a sample inlet (8) at one side of the mass spectrum detector (7) so as to be detected and identified.

7. The method of claim 6, wherein the swab assembly further comprises: the integral extraction time of the solid phase micro-extraction probe (1) is 5-30 minutes.

8. The method of claim 6, wherein the swab assembly further comprises: and after enriching the sample (3), the solid-phase micro-extraction probe (1) is immersed in pure water for 10-120 seconds to remove impurities attached to the surface, and then ionization is carried out.

9. The method of claim 6, wherein the swab assembly further comprises: the solid phase micro-extraction probe (1) is inserted into the capillary (6), and the distance between the spray head at the end part of the capillary (6) and the sample inlet (8) is 0.5-1.5 cm.

Technical Field

The embodiment of the invention relates to the field of separation and analysis devices and methods, in particular to a solid-phase micro-extraction swab device and a solid-phase micro-extraction swab method.

Background

The solid-phase micro-extraction technology is one of the most common sample pretreatment modes, is widely applied to the fields of food, natural products, medicine and health, clinical chemistry, biochemistry, toxicology, legal medicine and the like, and overcomes the defect that the traditional sample pretreatment technology is needed. The solid phase microextraction technology is a technology (reference documents [1] and [2]) for adsorbing and enriching substances to be detected in a sample through a solid phase microextraction coating on quartz fiber and concentrating analytes while extracting, and the solid phase microextraction probe after enriching the sample is combined with other analytical instruments such as a mass spectrum to realize sample detection (reference documents [3] and [4 ]). In the operation process of a common solid phase microextraction probe, the probe is directly placed into a liquid sample, and the probe is directly contacted with the sample to selectively adsorb and enrich target analytes.

However, for in-situ samples of human body, oral secretion, nasal secretion, skin secretion, etc., the traditional solid phase micro-extraction probe cannot be inserted into the human body for non-invasive sampling, and needs to collect the sample for enrichment (reference [5], such as collecting oral saliva, nasal mucus, etc., for human skin, the traditional solid phase micro-extraction probe lacks a liquid phase environment for extracting target analytes, and cannot extract solid surface samples.

The relevant documents proposed in the above background art are given below:

[1]Spietelun,A.；Pilarczyk,M.；Kloskowski,A.；Namiesnik,J.Chem Soc Rev2010,39,4524-4537.

[2]Eisert,R.；Pawliszyn,J.Crit Rev Anal Chem 1997,27,103-135.

[3]Fang,L.；Deng,J.W.；Yang,Y.Y.；Wang,X.W.；Chen,B.W.；Liu,H.T.；Zhou,H.Y.；Ouyang,G.F.；Luan,T.G.Trac-Trend Anal Chem2016,85,61-72.

[4]Vas,G.；Vekey,K.J Mass Spectrom 2004,39,233-254.

[5]Ouyang,G.F.；Vuckovic,D.；Pawliszyn,J.Chem Rev 2011,111,2784-2814.

disclosure of Invention

Therefore, the embodiment of the invention provides a solid phase micro-extraction swab device and a solid phase micro-extraction swab method, which solve the problem that solid and mucus cannot be directly enriched by solid phase micro-extraction at present by combining a solid phase micro-extraction probe and a sampling ball, dissolving a solid sample by sampling wetting and collecting a viscous sample.

In order to achieve the above object, the embodiments of the present invention provide the following technical solutions: a solid phase micro-extraction swab device and a method thereof comprise a solid phase micro-extraction probe and a sampling ball, wherein the sampling ball is wrapped outside the bottom end of the solid phase micro-extraction probe;

the bottom end of the solid phase micro-extraction probe is inserted into the sampling ball for sample enrichment, and is extracted from the sampling ball for further analysis of the enriched sample.

Further, the sampling ball is made of a porous, porous material that is wettable.

Further, the wettable, porous material is embodied as a fibrous material or a cotton ball.

Further, the sampling ball is used for wetting the sample, filtering impurities and isolating the probe while collecting the sample.

Further, the samples include liquid, mucus, and solid surface soluble samples.

The invention also provides a solid phase micro-extraction method of the solid phase micro-extraction swab device, which comprises the following steps:

step one, sampling: enriching the sample in the sampling ball by using a solid phase microextraction probe;

step two, ionization: putting one end of the solid phase micro-extraction probe after enriching the sample into a capillary tube pre-filled with a reagent for electrospray ionization;

step three, detection: and the sample generates ions and then enters a sample inlet at one side of the mass spectrum detector so as to be detected and identified.

Further, the overall extraction time of the solid phase micro-extraction probe is 5-30 minutes.

Further, after enriching the sample, the solid phase micro extraction probe is immersed in pure water for 10-120 seconds to remove impurities attached to the surface, and then ionization is performed.

Furthermore, the solid phase micro-extraction probe is inserted into the capillary, and the distance between the spray head at the end part of the capillary and the sample inlet is 0.5-1.5 cm.

The embodiment of the invention has the following advantages:

1. the sampling ball made of wettable loose porous materials is used as a sampler, so that viscous and particle impurities in the sample are filtered, analytes in liquid are more effectively enriched, the solid-phase microextraction probe is effectively isolated and protected, the sampling ball can be enriched in human samples such as oral cavities and nasal cavities of human bodies, and the sampling ball has wide market application prospect;

2. the invention uses the moist sampling ball for sampling, can realize the enrichment of the soluble analytes on the solid surface, the sample is dissolved on the sampling ball made of the cotton ball and is enriched, and the sampling and enrichment on the human skin are realized.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.

The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.

FIG. 1 is a schematic view of a solid-phase micro-extraction swab device according to a first embodiment of the present invention;

FIG. 2 is a schematic diagram of a solid phase microextraction swab coupled mass spectrometry in accordance with an embodiment of the present invention;

FIG. 3 is a first order mass spectrum of saliva analyzed in positive ion mode using the solid phase microextraction swab device of the present invention in accordance with example two;

FIG. 4 is a secondary mass spectrum of nicotine in saliva of a human body after smoke inhalation analyzed in positive ion mode using the solid phase microextraction swab device of the present invention in example two;

FIG. 5 is a first order mass spectrum of a second embodiment of the present invention using the solid phase microextraction swab device in positive ion mode;

FIG. 6 is a second mass spectrum of xylometazoline in the drug residue in the nasal cavity analyzed in positive ion mode using the solid phase microextraction swab device of the present invention in example two;

FIG. 7 is a first order mass spectrum of the second embodiment of the present invention using the wet solid phase microextraction swab device to analyze pesticide residue in human skin in positive ion mode;

FIG. 8 is a second mass spectrum of Dimethoate in pesticide residue in human skin analyzed in positive ion mode using the solid phase microextraction swab device of the present invention in example two;

in the figure: 1 solid phase micro extraction probe, 2 sampling ball, 3 sample, 4 reagent, 5 ion, 6 capillary, 7 mass spectrum detector, 8 mass spectrum sample inlet.

Detailed Description

The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.