CN105044161A - Method for discriminating furacilin and furazolidone in Tegillarca granosa by using electron nose - Google Patents

Abstract

The invention discloses a method for discriminating furacilin and furazolidone in Tegillarca granosa by using an electron nose. The method comprises the following steps: heating Tegillarca granosa soft tissues in a sample introduction bottle at 60DEG C to volatilize furacilin and furazolidone, setting appropriate array parameters of the sensor of an electron nose with the model of PEN3, obtaining the electric conductivity ratio of the sensor in the automatic mode identification system of the electron nose, and judging the Tegillarca granosa soft tissues contain furazolidone if the electric conductivity ratio parameter of a sensor No.2 is greater than 2.0; and judging the Tegillarca granosa soft tissues contain furacilin if the electric conductivity ratio parameter of a sensor No.2 is 0.68-0.71. The method for discriminating furacilin and furazolidone in Tegillarca granosa by using the electron nose has the advantages of simple detection, no extraction, no atlas analysis comparison, obvious discriminating result, good discriminating effect and short discriminating time.

Description

Electronic Nose is utilized to differentiate the method for nitrofurazone and furazolidone in mud blood clam

Technical field

The present invention relates to the discriminating of nitrofurazone and furazolidone, be specifically related to utilize Electronic Nose to differentiate the method for nitrofurazone and furazolidone in mud blood clam.

Background technology

Nitrofurazone (f μ gracilin) is a kind of antimicrobial of Prof. Du Yucang, can treat Animal diseases.Furazolidone (furazolidone, former name claims: furazolidone) is a kind of Nitrofuran antibiotics, and furazolidone is broad spectrum antibiotic, has inhibiting effect to common Gram-negative bacteria and positive bacteria.Nitrofurazone, furazolidone are all conventional furfuran compound, belong to persistence organic pollutant (PersistentOrganicPollutants, be called for short POPs), there is the very long half life period, and gather by food web, can be long-term retain in environment, to the existence that the threat of health all can be long-term.The detection of current furfuran compound in environment or biological sample generally first adopts: the chemical methodes such as supercritical fluid extraction (SFE), microwave radiation exaraction (MAE), accelerated solvent extraction (ASE), solid-phase microextraction (SPME) are extracted, then use the detections such as GC-MS(gas chromatography-mass spectrography) (GC-MS), Liquid Chromatography-Mass Spectrometry (LC-MS) or ELISA method; Extract and detect and separately carry out, detection of complex, differentiate that the time is long.Electronic Nose is made up of sensor array (No. 1-10) and automatic mode recognition system, can identify and detect volatile ingredient.It does not need to be separated volatile matter, can carry out express-analysis, have objective, evaluate smell accurately and quickly, and reproducible feature.Electronic Nose not only can carry out simple compare of analysis to the odiferous information of different sample, and can, by gathering standard specimen information building database and template, utilize statistical analysis technique to carry out qualitative and quantitative analysis to unknown sample.

Summary of the invention

Technical matters to be solved by this invention be to provide a kind of detect simple, the discriminating time is few, differentiate significantly to utilize Electronic Nose to differentiate the method for nitrofurazone and furazolidone in mud blood clam.

The present invention solves the problems of the technologies described above adopted technical scheme: utilize Electronic Nose to differentiate the method for nitrofurazone and furazolidone in mud blood clam, its step is as follows:

A, get after 1g mud blood clam soft tissue shreds, load in 15ml sample injection bottle, sample surfaces is 3/5 ~ 5/6 bottle height apart from bottleneck distance, and the soft lid of bottleneck seals, and at 60 DEG C of temperature, oscillation sample bottle 30min, cools 15min under room temperature;

B, open the sensor of model PEN3 Electronic Nose, preheating 30min, the sample introduction needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of sample introduction needle and bottleneck distance are 1/3 bottle height, again the air inlet needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of air inlet needle and bottleneck distance are greater than syringe needle and the bottleneck distance 1mm of sample introduction needle, then the array parameter setting this sensor detects: head space generation time 600s, hunting speed 500r/min, the total acquisition time 100s of signal, signal frequency 1.0s, lag time 600s, carrier gas is dried and clean air, air inflow is 300mL/min, flow rate of carrier gas 150mL/min, air inlet needle syringe needle is conducive to smell lower than sample introduction needle syringe needle and is gathered by sample introduction needle,

C, the automatic mode recognition system opening model PEN3 Electronic Nose are differentiated, if the Conductivity Ratio value parameter of No. 2 sensors is greater than 2.0, then mud blood clam soft tissue contains furazolidone, if the Conductivity Ratio value parameter of No. 2 sensors is 0.68 ~ 0.71, the Conductivity Ratio value parameter of No. 8 sensors is less than 0.9, then mud blood clam soft tissue contains nitrofurazone.

Compared with prior art, the invention has the advantages that the method utilizing Electronic Nose to differentiate nitrofurazone and furazolidone in mud blood clam, heated at 60 DEG C of temperature in sample injection bottle by mud blood clam soft tissue, nitrofurazone and furazolidone volatilization, use the array parameter that the sensor settings of the Electronic Nose of model PEN3 is suitable again, then the electrical conductivity ratio of sensor is obtained in the automatic mode recognition system of Electronic Nose, if the Conductivity Ratio value parameter of No. 2 sensors is greater than 2.0, then mud blood clam soft tissue contains furazolidone; If the Conductivity Ratio value parameter of No. 2 sensors is 0.68 ~ 0.71, then mud blood clam soft tissue contains nitrofurazone; Differentiate nitrofurazone and furazolidone in mud blood clam by Electronic Nose like this, detection method is simple, and do not need to extract, also know analyses and comparison well without figure, have identification result obvious, identification result is good, differentiates the advantage that the time is few.

Embodiment

Below in conjunction with embodiment, the present invention is described in further detail.

Embodiment 1

Electronic Nose is utilized to differentiate the method for nitrofurazone and furazolidone in mud blood clam, take off the shell that mud blood clam is hard, 1g is got after the part of softness being shredded, load in 15ml sample injection bottle, the mud blood clam parallel experiment of 5 Different sources (2, Qidong, Jiangsu plant, 3, Fenghua, Zhejiang plant), the soft lid sealing of bottleneck, screws bottle cap, simultaneously a blank sample injection bottle test.By each sample injection bottle all heating and thermal insulation 30min in 60 DEG C of waters bath with thermostatic control, 15min is cooled under room temperature, after making in bottle headspace gas balance, model PEN3 Electronic Nose (German Mecklenburg Airsense company) is utilized to detect, open the sensor (1-10 array) of the Electronic Nose of model PEN3, preheating 30min, the sample introduction needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of sample introduction needle and bottleneck distance are 1/3 bottle height, again the air inlet needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of air inlet needle and bottleneck distance are greater than the syringe needle of sample introduction needle and bottleneck distance 1mm(air inlet needle syringe needle and are conducive to smell lower than sample introduction needle syringe needle and are gathered by sample introduction needle), then the array parameter setting this sensor detects: head space generation time 600s, hunting speed 500r/min, the total acquisition time 100s of signal, signal frequency 1.0s, lag time 600s, carrier gas is dried and clean air, air inflow is 300mL/min, flow rate of carrier gas 150mL/min, the automatic mode recognition system opening the Electronic Nose of model PEN3 is differentiated, the Conductivity Ratio value parameter of No. 2 sensors of the mud blood clam of 2 plants in Qidong, Jiangsu is 0.68 ~ 0.71, the Conductivity Ratio value parameter 0.81 ~ 0.85 and 0.76 ~ 0.79 of No. 8 sensors, illustrates that mud blood clam soft tissue contains nitrofurazone, the Conductivity Ratio value parameter of No. 2 sensors of the mud blood clam of 3 plants in Fenghua, Zhejiang is respectively 2.21 ~ 2.25,2.87 ~ 2.93 and 3.01 ~ 3.05, illustrates that mud blood clam soft tissue contains furazolidone.

Embodiment 2

Preparing standard solution: furazolidone group: concentration 0.1 μ g/L, 1 μ g/L, 10 μ g/L, nitrofurazone group: concentration 0.1 μ g/L, 1 μ g/L, 10 μ g/L, blank group, then get 1mL and load 15ml sample injection bottle, sample injection bottle is heating and thermal insulation 30min in 60 DEG C of waters bath with thermostatic control, 15min is cooled under room temperature, open the sensor (1-10 array) of the Electronic Nose of model PEN3, preheating 30min, the sample introduction needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of sample introduction needle and bottleneck distance are 1/3 bottle height, again the air inlet needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of air inlet needle and bottleneck distance are greater than syringe needle and the bottleneck distance 1mm of sample introduction needle, then the array parameter setting this sensor detects: head space generation time 600s, hunting speed 500r/min, the total acquisition time 100s of signal, signal frequency 1.0s, lag time 600s, carrier gas is dried and clean air, air inflow is 300mL/min, flow rate of carrier gas 150mL/min, the automatic mode recognition system opening the Electronic Nose of model PEN3 is differentiated, the Conductivity Ratio value parameter of blank group No. 2 sensors is 1.0 ~ 1.3.The Conductivity Ratio value parameter of furazolidone group No. 2 sensors is: concentration 0.1 μ g/L, ratio parameter 3.01 ~ 4.12, concentration 1.0 μ g/L, ratio parameter 2.93 ~ 3.01, concentration 10. μ g/L, aspect ratio 2.72 ~ 2.87.The Conductivity Ratio value parameter of nitrofurazone group No. 2 sensors is all the Conductivity Ratio value parameter of 0.68 ~ 0.71, No. 8 sensors: concentration 0.1 μ g/L, ratio parameter 0.81 ~ 0.85, concentration 1.0 μ g/L, ratio parameter 0.79 ~ 0.81, concentration 10. μ g/L, ratio parameter 0.76 ~ 0.79.As can be seen from embodiment 1,2, furazolidone and nitrofurazone are distinguished obviously, and can scope quantitatively detect, and detect simple, fast.

Claims (1)

1. utilize Electronic Nose to differentiate the method for nitrofurazone and furazolidone in mud blood clam, it is characterized in that step is as follows:

A, get after 1g mud blood clam soft tissue shreds, load in 15ml sample injection bottle, sample surfaces is 3/5 ~ 5/6 bottle height apart from bottleneck distance, and the soft lid of bottleneck seals, and at 60 DEG C of temperature, oscillation sample bottle 30min, cools 15min under room temperature;

B, open the sensor of the Electronic Nose of model PEN3, preheating 30min, the sample introduction needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of sample introduction needle and bottleneck distance are 1/3 bottle height, again the air inlet needle of sensor is inserted in the soft lid of sample injection bottle, the syringe needle of air inlet needle and bottleneck distance are greater than syringe needle and the bottleneck distance 1mm of sample introduction needle, then the array parameter setting this sensor detects: head space generation time 600s, hunting speed 500r/min, the total acquisition time 100s of signal, signal frequency 1.0s, lag time 600s, carrier gas is dried and clean air, air inflow is 300mL/min, flow rate of carrier gas 150mL/min,

C, the automatic mode recognition system opening model PEN3 Electronic Nose are differentiated, if the Conductivity Ratio value parameter of No. 2 sensors is greater than 2.0, then mud blood clam soft tissue contains furazolidone, if the Conductivity Ratio value parameter of No. 2 sensors is 0.68 ~ 0.71, the Conductivity Ratio value parameter of No. 8 sensors is less than 0.9, then mud blood clam soft tissue contains nitrofurazone.