CN204925031U - Open -type ionizationoun atomizer - Google Patents
Open -type ionizationoun atomizer Download PDFInfo
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- CN204925031U CN204925031U CN201520632077.0U CN201520632077U CN204925031U CN 204925031 U CN204925031 U CN 204925031U CN 201520632077 U CN201520632077 U CN 201520632077U CN 204925031 U CN204925031 U CN 204925031U
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- Prior art keywords
- ion mobility
- glass capillary
- borosilicate glass
- capillary tube
- mobility spectrometry
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- 239000007921 spray Substances 0.000 claims abstract description 32
- 239000002184 metal Substances 0.000 claims abstract description 26
- 239000005388 borosilicate glass Substances 0.000 claims description 28
- 238000001871 ion mobility spectroscopy Methods 0.000 claims description 27
- 150000002500 ions Chemical class 0.000 abstract description 16
- 238000012360 testing method Methods 0.000 abstract description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract 2
- 229910052796 boron Inorganic materials 0.000 abstract 2
- 239000005368 silicate glass Substances 0.000 abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000000523 sample Substances 0.000 description 17
- 239000002537 cosmetic Substances 0.000 description 13
- 230000003115 biocidal effect Effects 0.000 description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- -1 fleraxacin Chemical compound 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 229940088710 antibiotic agent Drugs 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004949 mass spectrometry Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229960000282 metronidazole Drugs 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
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- 239000000203 mixture Substances 0.000 description 3
- IAIWVQXQOWNYOU-FPYGCLRLSA-N nitrofural Chemical compound NC(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 IAIWVQXQOWNYOU-FPYGCLRLSA-N 0.000 description 3
- 229960001907 nitrofurazone Drugs 0.000 description 3
- AYIRNRDRBQJXIF-NXEZZACHSA-N (-)-Florfenicol Chemical compound CS(=O)(=O)C1=CC=C([C@@H](O)[C@@H](CF)NC(=O)C(Cl)Cl)C=C1 AYIRNRDRBQJXIF-NXEZZACHSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- 206010012442 Dermatitis contact Diseases 0.000 description 2
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 description 2
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- 239000006035 Tryptophane Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229940097572 chloromycetin Drugs 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- VAOCPAMSLUNLGC-UHFFFAOYSA-N metronidazole Chemical compound CC1=NC=C([N+]([O-])=O)N1CCO VAOCPAMSLUNLGC-UHFFFAOYSA-N 0.000 description 2
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- NXFQHRVNIOXGAQ-YCRREMRBSA-N nitrofurantoin Chemical compound O1C([N+](=O)[O-])=CC=C1\C=N\N1C(=O)NC(=O)C1 NXFQHRVNIOXGAQ-YCRREMRBSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical compound C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- OTVAEFIXJLOWRX-NXEZZACHSA-N thiamphenicol Chemical compound CS(=O)(=O)C1=CC=C([C@@H](O)[C@@H](CO)NC(=O)C(Cl)Cl)C=C1 OTVAEFIXJLOWRX-NXEZZACHSA-N 0.000 description 2
- 229960003053 thiamphenicol Drugs 0.000 description 2
- 229960004799 tryptophan Drugs 0.000 description 2
- XUBOMFCQGDBHNK-JTQLQIEISA-N (S)-gatifloxacin Chemical compound FC1=CC(C(C(C(O)=O)=CN2C3CC3)=O)=C2C(OC)=C1N1CCN[C@@H](C)C1 XUBOMFCQGDBHNK-JTQLQIEISA-N 0.000 description 1
- KPQZUUQMTUIKBP-UHFFFAOYSA-N 1-(2-methyl-5-nitro-1-imidazolyl)-2-propanol Chemical compound CC(O)CN1C(C)=NC=C1[N+]([O-])=O KPQZUUQMTUIKBP-UHFFFAOYSA-N 0.000 description 1
- YZEUHQHUFTYLPH-UHFFFAOYSA-N 2-nitroimidazole Chemical compound [O-][N+](=O)C1=NC=CN1 YZEUHQHUFTYLPH-UHFFFAOYSA-N 0.000 description 1
- YVQVOQKFMFRVGR-VGOFMYFVSA-N 5-(morpholin-4-ylmethyl)-3-[(e)-(5-nitrofuran-2-yl)methylideneamino]-1,3-oxazolidin-2-one Chemical compound O1C([N+](=O)[O-])=CC=C1\C=N\N1C(=O)OC(CN2CCOCC2)C1 YVQVOQKFMFRVGR-VGOFMYFVSA-N 0.000 description 1
- VYDWQPKRHOGLPA-UHFFFAOYSA-N 5-nitroimidazole Chemical compound [O-][N+](=O)C1=CN=CN1 VYDWQPKRHOGLPA-UHFFFAOYSA-N 0.000 description 1
- XBHBWNFJWIASRO-UHFFFAOYSA-N 6-fluoro-1-(4-fluorophenyl)-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1=CC=C(F)C=C1 XBHBWNFJWIASRO-UHFFFAOYSA-N 0.000 description 1
- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 description 1
- DPSPPJIUMHPXMA-UHFFFAOYSA-N 9-fluoro-5-methyl-1-oxo-6,7-dihydro-1H,5H-pyrido[3,2,1-ij]quinoline-2-carboxylic acid Chemical compound C1CC(C)N2C=C(C(O)=O)C(=O)C3=C2C1=CC(F)=C3 DPSPPJIUMHPXMA-UHFFFAOYSA-N 0.000 description 1
- 208000002874 Acne Vulgaris Diseases 0.000 description 1
- SPFYMRJSYKOXGV-UHFFFAOYSA-N Baytril Chemical compound C1CN(CC)CCN1C(C(=C1)F)=CC2=C1C(=O)C(C(O)=O)=CN2C1CC1 SPFYMRJSYKOXGV-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 206010015150 Erythema Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- NTAFJUSDNOSFFY-UHFFFAOYSA-N Ipronidazole Chemical compound CC(C)C1=NC=C([N+]([O-])=O)N1C NTAFJUSDNOSFFY-UHFFFAOYSA-N 0.000 description 1
- XAGMUUZPGZWTRP-ZETCQYMHSA-N LSM-5745 Chemical compound C([C@@H](N1C2=C(C(C(C(O)=O)=C1)=O)C=C1F)C)OC2=C1C1(N)CC1 XAGMUUZPGZWTRP-ZETCQYMHSA-N 0.000 description 1
- BPFYOAJNDMUVBL-UHFFFAOYSA-N LSM-5799 Chemical compound C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3N(C)COC1=C32 BPFYOAJNDMUVBL-UHFFFAOYSA-N 0.000 description 1
- IPWKIXLWTCNBKN-UHFFFAOYSA-N Madelen Chemical compound CC1=NC=C([N+]([O-])=O)N1CC(O)CCl IPWKIXLWTCNBKN-UHFFFAOYSA-N 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- HJLSLZFTEKNLFI-UHFFFAOYSA-N Tinidazole Chemical compound CCS(=O)(=O)CCN1C(C)=NC=C1[N+]([O-])=O HJLSLZFTEKNLFI-UHFFFAOYSA-N 0.000 description 1
- 206010000496 acne Diseases 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 230000003255 anti-acne Effects 0.000 description 1
- 150000003851 azoles Chemical class 0.000 description 1
- 235000013532 brandy Nutrition 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SOROIESOUPGGFO-UHFFFAOYSA-N diazolidinylurea Chemical compound OCNC(=O)N(CO)C1N(CO)C(=O)N(CO)C1=O SOROIESOUPGGFO-UHFFFAOYSA-N 0.000 description 1
- 229960001083 diazolidinylurea Drugs 0.000 description 1
- NOCJXYPHIIZEHN-UHFFFAOYSA-N difloxacin Chemical compound C1CN(C)CCN1C(C(=C1)F)=CC2=C1C(=O)C(C(O)=O)=CN2C1=CC=C(F)C=C1 NOCJXYPHIIZEHN-UHFFFAOYSA-N 0.000 description 1
- 229950001733 difloxacin Drugs 0.000 description 1
- 229960000946 dimetridazole Drugs 0.000 description 1
- IBXPYPUJPLLOIN-UHFFFAOYSA-N dimetridazole Chemical compound CC1=NC=C(N(=O)=O)N1C IBXPYPUJPLLOIN-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000132 electrospray ionisation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960002549 enoxacin Drugs 0.000 description 1
- IDYZIJYBMGIQMJ-UHFFFAOYSA-N enoxacin Chemical compound N1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 IDYZIJYBMGIQMJ-UHFFFAOYSA-N 0.000 description 1
- 229960000740 enrofloxacin Drugs 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 231100000321 erythema Toxicity 0.000 description 1
- 229960000702 flumequine Drugs 0.000 description 1
- 229950000337 furaltadone Drugs 0.000 description 1
- 229960001625 furazolidone Drugs 0.000 description 1
- PLHJDBGFXBMTGZ-WEVVVXLNSA-N furazolidone Chemical compound O1C([N+](=O)[O-])=CC=C1\C=N\N1C(=O)OCC1 PLHJDBGFXBMTGZ-WEVVVXLNSA-N 0.000 description 1
- 229960003923 gatifloxacin Drugs 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229960002422 lomefloxacin Drugs 0.000 description 1
- ZEKZLJVOYLTDKK-UHFFFAOYSA-N lomefloxacin Chemical compound FC1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNC(C)C1 ZEKZLJVOYLTDKK-UHFFFAOYSA-N 0.000 description 1
- 229960002531 marbofloxacin Drugs 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229960003702 moxifloxacin Drugs 0.000 description 1
- FABPRXSRWADJSP-MEDUHNTESA-N moxifloxacin Chemical compound COC1=C(N2C[C@H]3NCCC[C@H]3C2)C(F)=CC(C(C(C(O)=O)=C2)=O)=C1N2C1CC1 FABPRXSRWADJSP-MEDUHNTESA-N 0.000 description 1
- 229960003808 nadifloxacin Drugs 0.000 description 1
- JYJTVFIEFKZWCJ-UHFFFAOYSA-N nadifloxacin Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)CCC3=C1N1CCC(O)CC1 JYJTVFIEFKZWCJ-UHFFFAOYSA-N 0.000 description 1
- 229960001180 norfloxacin Drugs 0.000 description 1
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 description 1
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- FHFYDNQZQSQIAI-UHFFFAOYSA-N pefloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCN(C)CC1 FHFYDNQZQSQIAI-UHFFFAOYSA-N 0.000 description 1
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- 238000002203 pretreatment Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- PQFRTXSWDXZRRS-UHFFFAOYSA-N ronidazole Chemical compound CN1C(COC(N)=O)=NC=C1[N+]([O-])=O PQFRTXSWDXZRRS-UHFFFAOYSA-N 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229950007734 sarafloxacin Drugs 0.000 description 1
- 229960004076 secnidazole Drugs 0.000 description 1
- 229960004954 sparfloxacin Drugs 0.000 description 1
- DZZWHBIBMUVIIW-DTORHVGOSA-N sparfloxacin Chemical compound C1[C@@H](C)N[C@@H](C)CN1C1=C(F)C(N)=C2C(=O)C(C(O)=O)=CN(C3CC3)C2=C1F DZZWHBIBMUVIIW-DTORHVGOSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The utility model discloses an open -type ionizationoun atomizer, including ion mobility register for easy reference host computer (1), metal microelectrode (2), boron silicate glass capillary (3), support (4), metal clip (5), power cord (6) and safety interlock (7), ion mobility register for easy reference host computer (1) is including the electron spray introduction port electron spray introduction port department is provided with lens, the front end setting of boron silicate glass capillary (3) is being close to the lens part, the rear end with the front end of metal microelectrode (2) links to each other, the rear end of metal microelectrode (2) respectively with support (4) and metal clip (5) link to each other, metal clip (5) are passed through power cord (6) with the high voltage output interface of ion mobility register for easy reference host computer (1) links to each other. Open -type ionizationoun atomizer be the improvement of going on on ion mobility register for easy reference basis, the testing result is accurate, reliable.
Description
Technical field
The utility model relates to pick-up unit, particularly relates to the open type ionizing spray device used in 40 kinds of violated antibiotic methods in a kind of ion mobility spectrometry rapid screening cosmetics.
Background technology
Microbiotic is a class prescription medicine, and Long-Time Service, can cause the bad reactions such as contact dermatitis, shows as erythema, oedema, erosion, furfur, oozes out, itch, scorching hot etc.China's " cosmetics health specification " (version in 2007) specifies, antibiotics composition is cosmetics forbidding component, and European Union also specifies this must not add microbiotic in cosmetics.Therefore, in cosmetics, add microbiotic and belong to unlawful practice.
Carbostyril antibiotic, Nitrofuran antibiotics, chloromycetin series antibiotics and nitroimidazole antibiotics all belong to the four class microbiotic easily added in cosmetics, antibiotic composition is added in cosmetics, obviously can improve it except mite, anti-acne effect, to trichocryptosis, acne, brandy nose also has certain curative effect, but Long-Time Service or contact Diazolidinyl Urea, cause fash, allergy or contact dermatitis, bad reaction is caused to central nervous system and enteron aisle, even exist carcinogenic, the possibility of teratogenesis tire, the drug resistance of microorganism can be caused time serious, cause healthy hidden danger.
And in prior art, lack the antibiotic pick-up unit that can detect these fast and be harmful to.
Utility model content
The technical problems to be solved in the utility model is to provide a kind of open type ionizing spray device.
A kind of open type ionizing spray device, comprises ion mobility spectrometry main frame, metal microelectrode, borosilicate glass capillary tube, support, metal clip, power lead and safety interlock; Described ion mobility spectrometry main frame comprises electric spray sample introduction mouth, described electric spray sample introduction mouth place is provided with lens, the front end of described borosilicate glass capillary tube is arranged near described lens part, rear end is connected with the front end of described metal microelectrode, the rear end of described metal microelectrode is connected with described metal clip with described support respectively, and described metal clip is connected with the High voltage output interface of described ion mobility spectrometry main frame by described power lead; Described safety interlock is arranged on described ion mobility spectrometry main frame, and near described electric spray sample introduction mouth; The length of described borosilicate glass capillary tube is 5cm.
Open type ionizing spray device described in the utility model, the internal diameter that the front end of wherein said borosilicate glass capillary tube is namely most advanced and sophisticated is 5 ~ 15 μm, and the rear end external diameter of described borosilicate glass capillary tube is 1.5mm, and internal diameter is 0.86mm.
Open type ionizing spray device described in the utility model, the distance between the front end of wherein said borosilicate glass capillary tube and described lens is 3 ~ 5mm.
The utility model open type ionizing spray device difference from prior art is:
When adopting the utility model open type ionizing spray device to carry out antibiotic detection, without the need to sample pre-treatments, under atmospheric pressure open type environment, realize sample ionization, the rapid screening adopting Ion mobility spectrometry to carry out microseconds time-scale detects; Violated antibiotic sample is detected for the examination of employing ion mobility spectrometry, adopts High Performance Liquid Chromatography/Mass Spectrometry/mass spectroscopy to confirm further.Adopt device of the present utility model to detect, accurately, reliably, while guaranteeing to detect data accuracy, greatly reduce testing cost, improve detection efficiency; Device in the utility model is the improvement carried out on the basis of original ion mobility spectrometry, is more suitable for the antibiotic detection in cosmetics.
Below in conjunction with accompanying drawing, open type ionizing spray device of the present utility model is described further.
Accompanying drawing explanation
Fig. 1 is the one-piece construction schematic diagram of open type ionizing spray device in the utility model;
Fig. 2 is the structural representation of the major part of open type ionizing spray device in the utility model;
Fig. 3 is the partial enlarged drawing in Tu2Zhong T district.
Embodiment
Embodiment 1
As shown in Figure 1-Figure 3, open type ionizing spray device comprises ion mobility spectrometry main frame 1, and (ion mobility spectrometry instrument comprises ion mobility spectrometry main frame 1 and ion gun, ion gun is arranged on the electric spray sample introduction mouth place of ion mobility spectrometry main frame 1, and ion mobility spectrometry main frame of the present utility model 1 is for removing ionogenic ion mobility spectrometry instrument), metal microelectrode 2, borosilicate glass capillary tube 3, support 4, metal clip 5, power lead 6 and safety interlock 7; Ion mobility spectrometry main frame 1 comprises electric spray sample introduction mouth, at electric spray sample introduction mouth, place is provided with lens, the front end of borosilicate glass capillary tube 3 is arranged near lens part, rear end is connected with the front end of metal microelectrode 2, the rear end of metal microelectrode 2 is connected with metal clip 5 with support 4 respectively, and metal clip 5 is connected with the High voltage output interface of ion mobility spectrometry main frame 1 by power lead 6; Safety interlock 7 is arranged on ion mobility spectrometry main frame 1, and near electric spray sample introduction mouth.The internal diameter that the front end of borosilicate glass capillary tube 3 is namely most advanced and sophisticated is 5 ~ 15 μm; Distance between the front end of borosilicate glass capillary tube 3 and lens is 3 ~ 5mm.The length of described borosilicate glass capillary tube 3 is 5cm.The rear end external diameter of described borosilicate glass capillary tube 3 is 1.5mm, and internal diameter is 0.86mm.
High-tension electricity by the solution ejection in borosilicate glass capillary tube 3, forms charged spray by metal microelectrode 2, spray enter migration tube front end through lens go to solution district.
Borosilicate glass capillary tube 3 adopts standard wall borosilicate glass blank and microelectrode to draw instrument and prepares, and the specification of standard wall borosilicate glass blank is external diameter is 1.5mm, and internal diameter is 0.86mm; Concrete preparation method comprises the steps: that standard wall borosilicate glass blank being placed in microelectrode draws instrument, the parameters that microelectrode draws instrument is set, prepare borosilicate glass capillary tube 3, the parameters that microelectrode draws instrument is set to: heating-up temperature 450 DEG C, value of thrust 0 newton, speed 5 DEG C/sec, circulation time 1 second, air pressure 60,000 handkerchief.
Device of the present utility model is adopted to detect the microbiotic in cosmetics:
One, instrument and device
Ion mobility spectrometry main frame (EXCELLIMS company of the U.S., model is GA2100, front tryptophane and citric acid is used to rectify an instrument under negative ions pattern respectively), comprise ion fence gate controller, air filter, high resolving power Ion transfer analyzer, Faraday cup detecting device, instrument controlling and data handling system; Standard wall borosilicate glass blank (external diameter 1.5mm, internal diameter 0.86mm); Microelectrode draws instrument (SUTTER company of the U.S., model is P-1000).
Two, reagent and material
Methyl alcohol and acetonitrile (Fisher company of the U.S.) and formic acid (Sigma-Aldrich) are chromatographically pure, tryptophane and citric acid (U.S. Sigma-Aldrich is made into 10 μ g/mL with methyl alcohol and carries out instrumental correction), 40 kinds of violated microbiotic (acidum nalidixicums, flumequine, Dan Nuosha star, marbofloxacin, Lomefloxacin, Sparfloxacin, Pazufloxacin, Nadifloxacin, Ciprofloxacin, MOXIFLOXACIN, Ofloxacin, Difloxacin, gatifloxacin, Pefloxacin, Norfloxacin, fleraxacin, sarafloxacin, Enoxacin, Enrofloxacin, furazolidone, furaltadone, furantoin, nitrofurazone, chloromycetin, Thiamphenicol, Florfenicol, 4-nitroimidazole, 2-metronidazole, hydroxyl metronidazole, metronidazole, Dimetridazole, MCMN, special azoles of rattling away, chlorine metronidazole, benzene nitre imidazoles, secnidazole, Tinidazole, hydroxyl ipronidazole, Ornidazole and ipronidazole, purity is all greater than 93%, German Dr.Ehrenstorfer and Fluka company) with methyl alcohol or acetonitrile (containing 0.1% formic acid, furantoin, nitrofurazone, chloromycetin, except Thiamphenicol and Florfenicol) be the standard reserving solution of solvent preparation 1mg/mL, be diluted to 10 μ g/mL with homogeneous solvent during analytical test.
Three, experimental technique:
Employing ion mobility spectrometry detects: dip cosmetic sample with metal microelectrode 2, insert in advance by the borosilicate glass capillary tube that methyl alcohol fills, be positioned over the electric spray sample introduction mouth front end of ion mobility spectrometry main frame, setting ion mobility spectrometry host parameter, sample is through ionization, enter after migration tube is separated and detect through Faraday cup detecting device, obtain corresponding collection of illustrative plates.
The sampling amount of cosmetic sample is 1mg, and in borosilicate glass capillary tube, the charging amount of methyl alcohol is 10 μ L; Methyl alcohol need fill the tip to borosilicate glass capillary tube 3, and can not produce bubble.
Ion mobility spectrometry host parameter is set as:
Source voltage (V): 1900 (electron spray positive ion mode)/1834 (Negative electrospray ionization pattern);
Migration tube voltage (V): 8000;
Migration tube temperature (DEG C): 180;
Gas preheater temperature (DEG C): 180;
Spectrum width (ms): 26;
Ion fence gate pulse width (μ s): 59;
Ion fence gate voltage (V): 30;
Drift gas velocity (L/min): 1.50;
Off-gas pump flow velocity (L/min): 0.66.
The chemical abstracts numbering of table 140 kind of violated antibiotic medicine, feature transit time and detection limit
Violated antibiotic sample is detected for the examination of employing ion mobility spectrometry, adopts High Performance Liquid Chromatography/Mass Spectrometry/mass spectroscopy to confirm further.40 kinds of violated antibiotic chemical abstracts numberings, precursor ion, product ion, taper hole voltage and collision energies are as shown in table 2:
The chemical abstracts numbering of table 240 kind of violated antibiotic medicine, precursor ion, product ion, taper hole voltage and collision energy
Four, results and analysis
1, the making of kapillary is extracted
The making key of borosilicate extraction kapillary is the size that its most advanced and sophisticated internal diameter draws, and internal diameter too conference causes sample spray effect poor, and Ionization Efficiency is low, thus has a strong impact on target substance sensitivity; Too little, easily cause tip clogs, sample solution is difficult to ejection, causes instrumental sensitivity to decline even no signal equally.Therefore, the utility model draws the key parameter of instrument by optimizing microelectrode, as heating-up temperature and speed etc., draw a series of kapillary, calculate its most advanced and sophisticated inner diameter values under an optical microscope, select the kapillary of most advanced and sophisticated 5-15 μm of internal diameter size as extraction spraying source, to reach optimum ionisation effect.
2, detection limit and accuracy
Under experiment optimal condition, quantitative test is carried out to 40 kinds of violated microbiotic.In blank cosmetic sample, add the violated microbiotic of a series of different quality concentration, then carrying out analysis according to the utility model method and measure, is the detection limit of each material of 3 calculating by signal to noise ratio (S/N ratio), in table 1.Adopt the accuracy of the recovery testu method of inspection, the recovery of standard addition of 40 kinds of violated antibiotic substance, all more than 80%, shows that the method has good accuracy.
3, the examination of positive is made by oneself
In cosmetics, quantitatively add the microbiotic standard items of different quality concentration, fully mix, and leave standstill 1 hour, obtained positive, carry out analysis and measure.
Above-described embodiment is only be described preferred implementation of the present utility model; not scope of the present utility model is limited; under the prerequisite not departing from the utility model design spirit; the various distortion that those of ordinary skill in the art make the technical solution of the utility model and improvement, all should fall in protection domain that the utility model claims determine.
Claims (3)
1. an open type ionizing spray device, is characterized in that: comprise ion mobility spectrometry main frame (1), metal microelectrode (2), borosilicate glass capillary tube (3), support (4), metal clip (5), power lead (6) and safety interlock (7); Described ion mobility spectrometry main frame (1) comprises electric spray sample introduction mouth, described electric spray sample introduction mouth place is provided with lens, the front end of described borosilicate glass capillary tube (3) is arranged near described lens part, rear end is connected with the front end of described metal microelectrode (2), the rear end of described metal microelectrode (2) is connected with described metal clip (5) with described support (4) respectively, and described metal clip (5) is connected by the High voltage output interface of described power lead (6) with described ion mobility spectrometry main frame (1); Described safety interlock (7) is arranged on described ion mobility spectrometry main frame (1), and near described electric spray sample introduction mouth; The length of described borosilicate glass capillary tube (3) is 5cm.
2. open type ionizing spray device according to claim 1, it is characterized in that: the internal diameter that the front end of described borosilicate glass capillary tube (3) is namely most advanced and sophisticated is 5 ~ 15 μm, the rear end external diameter of described borosilicate glass capillary tube (3) is 1.5mm, and internal diameter is 0.86mm.
3. open type ionizing spray device according to claim 2, is characterized in that: the distance between the front end of described borosilicate glass capillary tube (3) and described lens is 3 ~ 5mm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| CN105606688A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of chloramphenicol and metronidazole in cosmetics |
| CN105675707A (en) * | 2016-01-14 | 2016-06-15 | 中国检验检疫科学研究院 | Rapid detection method of bisphenol A in liquid milk |
| CN105699474A (en) * | 2016-01-14 | 2016-06-22 | 中国检验检疫科学研究院 | Rapid detection method for epitestosterone in liquid cosmetic |
| CN107121487A (en) * | 2017-07-05 | 2017-09-01 | 中国检验检疫科学研究院 | A kind of normal pressure velocity of sound electrospray ionization device and its application |
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- 2015-08-20 CN CN201520632077.0U patent/CN204925031U/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105606689A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of di(2-ethylhexyl) phthalate in beverages |
| CN105606688A (en) * | 2016-01-14 | 2016-05-25 | 中国检验检疫科学研究院 | Quick detection method of chloramphenicol and metronidazole in cosmetics |
| CN105675707A (en) * | 2016-01-14 | 2016-06-15 | 中国检验检疫科学研究院 | Rapid detection method of bisphenol A in liquid milk |
| CN105699474A (en) * | 2016-01-14 | 2016-06-22 | 中国检验检疫科学研究院 | Rapid detection method for epitestosterone in liquid cosmetic |
| CN107121487A (en) * | 2017-07-05 | 2017-09-01 | 中国检验检疫科学研究院 | A kind of normal pressure velocity of sound electrospray ionization device and its application |
| CN107121487B (en) * | 2017-07-05 | 2019-10-01 | 中国检验检疫科学研究院 | A kind of normal pressure velocity of sound electrospray ionization device and its application |
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