CN1195218C - Detection device of benzoperoxide in flour and detection method - Google Patents
Detection device of benzoperoxide in flour and detection method Download PDFInfo
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- CN1195218C CN1195218C CNB03114697XA CN03114697A CN1195218C CN 1195218 C CN1195218 C CN 1195218C CN B03114697X A CNB03114697X A CN B03114697XA CN 03114697 A CN03114697 A CN 03114697A CN 1195218 C CN1195218 C CN 1195218C
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Abstract
The present invention relates to a detecting device for benzoyl peroxide in flour, which comprises a pressure increasing apparatus, a valve or a switch, a pressure regulator, a sample pool, a micro-light measurer, a controller and a computer, wherein the micro-light measurer is in communication with the sample pool by a capillary tube. The device has the advantages of reasonable design, high sensitivity, accuracy, rapidness, high accuracy of detecting results, etc. A detecting method for benzoyl peroxide in flour of the present invention comprises the following steps: preparing 0.1 mol/L of sodium bicarbonate-sodium hydroxide buffer solution, preparing a light emitting reagent, preparing the standard solution of benzoyl peroxide, preparing detected sample solution, making a standard curve and detecting the benzoyl peroxide. The detecting method has the advantages of high detecting sensitivity, accuracy, rapidness, convenience, stability, etc. The detecting device and the detecting method of the present invention can be used for detecting benzoyl peroxide in flour, and can also be used for detecting benzoyl peroxide in vegetable oil and food.
Description
Technical field
The invention belongs to by means of the chemistry of measuring material or physical property is tested or analysis of material and with per-compound additive material processing flour or dough/pasta technical field, be specifically related to the determinator and the detection method of benzoyl peroxide in the flour.
Background technology
Benzoyl peroxide is a kind of flour improver, and it can make, and xenthophylls destroys and the increase whiteness in the flour.As far back as the '20s in last century, the Dutchman just is used for benzoyl peroxide the bleaching of flour, the quality of improvement flour.China recent years is brought into use, but the excess of benzoyl peroxide uses the vitamin that will make in the flour by considerable damage, reduced the absorption of human body to vitamin, poisonous substances such as its decomposition product benzoic acid, phenol detoxify in the human liver simultaneously, the people of and liver dysfunction weak for liver function, because of its bio-transformation miopragia, detoxification ability reduces, cause hepatic disease, even bring out liver cancer.Therefore add benzoyl peroxide and too much be unfavorable for the healthy of people in flour, Gu Geguo has stipulated its limit standard.States such as American and Britain fill the maximum of using benzoyl peroxide perhaps in flour and are 0.05g/kg, China " food additives use hygienic standard " of revision in 1996 (GB2760-96) in the regulation flour benzoyl peroxide maximum use amount be 0.06g/kg.
At present, benzoyl peroxide pick-up unit and detection method, the much more external extracted by ether that adopt are carried out colorimetric method for determining or gas chromatography determination after being reduced to benzoic acid.Above method need be carried out removal of impurities formality repeatedly, complex operation, and minute is long.The method of domestic present employing generally is to use high effective liquid chromatography for measuring after benzoyl peroxide is reduced to benzoic acid.Recently, have the research report directly to measure benzoyl peroxide, but this method sensitivity is not high and required instrument costliness, is difficult to promote with high performance liquid chromatography.Chemoluminescence method once was used to detect the peroxide lipid material, but method needs cromoci to make catalyzer, and the content that detects benzoyl peroxide in the flour with this method does not appear in the newspapers.
Traditional chemiluminescence analysis has discrete sampling and flow injection type dual mode, and relative merits are respectively arranged.The flow injection sampling system is owing to existing diffusion phenomena to cause dilution effect in the sample injection process, thereby the sensitivity of measuring is affected, and the measurement of discrete sampling method is total luminous signal, need not the liquid current-carrying during sample introduction again, avoid the dilution effect that causes owing to the sample diffusion phenomenon in the flow injection method sample introduction process effectively, thereby had higher mensuration sensitivity.Because in all chemiluminescence reactions, chemiluminescence intensity all is the function of time, and manyly all belongs to rapid reaction, and 1 second of reaction beginning is with the interior luminescence peak that reaches, and decay rapidly.Thereby in the discrete sampling method, to obtain high sensitivity and reappearance, and the application of sample amount must be accurately, and application of sample speed must be fast and constant.Present instrument both domestic and external all is employing hand sampling or electrokinetic injection method, and speed and sample size are difficult to accurately control, and is just difficult more to the sample of micro updating especially.Also be difficult for being implemented in line analysis in addition.
Summary of the invention
Technical matters to be solved by this invention is to provide the pick-up unit of benzoyl peroxide in a kind of flour.
Another technical matters to be solved by this invention is to provide the detection method of benzoyl peroxide in a kind of flour.
The pick-up unit that solves the problems of the technologies described above the technical scheme that is adopted and be benzoyl peroxide in the flour of the present invention comprises:
Compressed-air actuated gas cylinder can be provided.Be provided with manometric pressure regulator.Be arranged on valve or switch on the pipeline that links between gas cylinder and the pressure regulator.The top is provided with the sample cell that gland bonnet can hold detected sample solution, and this sample cell links by pipeline and pressure regulator.The low-light-level measurement device that links by kapillary and sample cell, this low-light-level measurement device comprises: low-light-level measurement device housing, left end cap, power-line terminal, photomultiplier, the chemiluminescence reaction pond, feed tube, the feed liquor switch, right end cap, the removal waste fluid pipe, the removal waste fluid switch, the signal output wiring terminal, left end cap is arranged on the left end of low-light-level measurement device housing, right end cap is arranged on the right-hand member of low-light-level measurement device housing, the chemiluminescence reaction pond is arranged on right side in the low-light-level measurement device housing, photomultiplier is arranged on left side in the low-light-level measurement device housing, sample outlet end capillaceous penetrates and is arranged on top, chemiluminescence reaction pond in the low-light-level measurement device housing, feed tube is arranged on chemiluminescence reaction pond top and passes low-light-level measurement device housing and link with the feed liquor switch that is installed on the feed tube, removal waste fluid pipe and chemiluminescence reaction pond link and pass low-light-level measurement device housing and link with the removal waste fluid switch that is installed on the removal waste fluid pipe, and the power-line terminal that is arranged on the left end cap is connected with photomultiplier by lead with the signal output wiring terminal.It comprises the controller that is used to control the low-light-level measurement device, and this controller is connected with the low-light-level measurement device by cable or wire.It also comprises the computing machine that is used to carry out data processing, and this computing machine is connected with the signal output wiring terminal by cable.
Chemiluminescence reaction of the present invention pond is to make with the organic or inorganic transparent material.
The horizontal section in chemiluminescence reaction of the present invention pond is a rectangle.
The present invention's internal diameter capillaceous is 50 μ m or 75 μ m or 100 μ m.
Kapillary of the present invention is to make with silica glass material.
The detection method of using apparatus of the present invention to carry out benzoyl peroxide in the flour comprises the steps:
(1) 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution preparation
Compound method is mixed with 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution routinely.
(2) luminescence reagent preparation
The luminol or derivatives thereof is prepared into luminescence reagent according to a conventional method with 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution.
(3) preparation of benzoyl peroxide standard solution
Take by weighing benzoyl peroxide 25mg, add in the 25mL volumetric flask, be settled to scale mark with absolute ethyl alcohol, being prepared into concentration is the standard stock solution of the benzoyl peroxide of 1mg/mL, places in the refrigerator and preserves, and uses the absolute ethyl alcohol stepwise dilution during use.
(4) detected sample liquid preparation
Take by weighing commercially available flour 0.1g, move in the centrifuge tube, add the 5mL absolute ethyl alcohol, mixing and stirring, placed 10 minutes, and on hydro-extractor centrifugal 5 minutes, filtered with the rotating speed of 4000r/min, filter residue extracts 2 times with identical method, is settled to 25mL with absolute ethyl alcohol behind the merging filtrate, shakes up.
(5) making of typical curve
Standard stock solution with absolute ethyl alcohol stepwise dilution benzoyl peroxide is mixed with concentration 6.0 * 10
-10～1.0 * 10
-6Benzoyl peroxide standard solution in the g/mL scope, to be settled to scale mark, open the feed liquor switch of low-light-level measurement device upper end, add 1～3mL luminescence reagent in the chemiluminescence reaction pond, getting 1～3mL benzoyl peroxide standard solution with the little centrifuge tube of tygon places in the sample cell, sample introduction end capillaceous inserts in the sample solution, upper end cover top cover labyrinth at sample cell, open the switch and the valve of gas cylinder, the gas outlet pressure of regulating pressure regulator is 4kpa, benzoyl peroxide standard solution in the sample cell carries out chemical reaction with luminescence reagent in kapillary splashes into the chemiluminescence reaction pond of low-light-level measurement device, regulating the photomultiplier negative high voltage is 800v, gain is 1, measuring the values of chemiluminescence of each solution, is horizontal ordinate with the concentration of benzoyl peroxide standard solution, and chemiluminescence intensity is an ordinate relatively, with computing machine drawing standard curve, its equation of linear regression is:
I
cl＝4.65(×10
9g/mL)C+8.28
Correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration of benzoyl peroxide, and unit is g/mL, and detecting of benzoyl peroxide is limited to 1.4 * 10
-10G/mL.
(6) detection of benzoyl peroxide
Open the feed liquor switch of low-light-level measurement device upper end, add 1～3mL luminescence reagent in the chemiluminescence reaction pond, getting the detected flour sample solution of 1～3mL with the little centrifuge tube of tygon places in the sample cell, sample introduction end capillaceous inserts in the sample solution, upper end cover top cover labyrinth at sample cell, open the switch and the valve of gas cylinder, the gas outlet pressure of regulating pressure regulator is 4kpa, sample solution in the sample cell carries out chemical reaction with luminescence reagent in kapillary splashes into the chemiluminescence reaction pond of low-light-level measurement device, the negative high voltage of regulating photomultiplier is 800v, gain is 1, and computing machine is pressed equation of linear regression:
I
cl＝4.65(×10
9g/mL)C+8.28
Correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration of benzoyl peroxide, and the content that COMPUTER CALCULATION goes out benzoyl peroxide in the flour is 2.5 * 10
8C, unit are mg/Kg.
Pick-up unit of the present invention with the fine inner diameter kapillary as analytic sample passage and sample injector, with gaseous tension as sample solution sample introduction expulsive force, sample solution carries out chemiluminescence reaction with luminescence reagent in the chemiluminescence reaction pond, photoelectric sensor converts the chemiluminescence signal that receives to electric signal and outputs to computing machine, by computing machine the electric signal of importing is carried out data processing and demonstrates testing result.Apparatus of the present invention adopted the less kapillary of internal diameter and fix its length and definite gaseous tension after automatically drip sample, the time interval between the sample drop that the kapillary port produces is 20 seconds, but per minute sample introduction three times, be convenient to automatic sampling, simultaneously also shortened the sample determination time, and the volume equal and opposite in direction that each drop drips promptly drips the sample amount at every turn and equates, thereby luminous favorable reproducibility.The range of linearity that apparatus of the present invention detect benzoyl peroxide is 5 * 10
-10～1 * 10
-6G/mL, detection limit reaches 1.4 * 10
-10G/mL exceeds 3～4 orders of magnitude of detection limit of bibliographical information, to 2.0 * 10
-8The relative standard deviation (RSD) of 11 replicate determinations of benzoyl peroxide standard solution of g/mL is 1.5%.The sample recovery of standard addition is 97%～103%.Benzoyl peroxide is directly with the absolute ethyl alcohol extraction and determination in the flour, and common coexistence component is noiseless.Sample feeding amount and luminescence-producing reaction agent solution consumption are few, drip sample automatically, have shortened the sample determination time, detect fast luminous favorable reproducibility.It has reasonable in design, highly sensitive, accurate, quick, testing result degree of accuracy advantages of higher, can be used for the detection of benzoyl peroxide in the flour, also can be used for the detection of benzoyl peroxide in vegetable oil and the food.
Detection method of the present invention is compared with discrete sampling formula chemoluminescence method and portable injection chemiluminescence method, owing to need not current-carrying during sample introduction, avoid sample diffusion phenomenon and the dilution effect followed in the portable injection chemiluminescence method sample introduction process effectively, improved the sensitivity of measuring.It has advantages such as detection sensitivity is higher, accurate, quick, easy, stable, can be used for the detection of benzoyl peroxide in the flour, also can be used for the detection of benzoyl peroxide in vegetable oil and the food.
Description of drawings
Fig. 1 is the structural representation of an embodiment of pick-up unit of benzoyl peroxide in the flour of the present invention.
Fig. 2 is the front view of low-light-level measurement device 2 among Fig. 1.
Fig. 3 is the cut-open view of Fig. 2.
Fig. 4 is the right view of Fig. 1.
Fig. 5 is the cut-open view of chemiluminescence reaction pond 2-5 among Fig. 3.
Fig. 6 is the vertical view of Fig. 5.
Fig. 7 is the precision figure of detection method of the present invention.
Embodiment
The present invention is described in more detail below in conjunction with drawings and Examples, but the invention is not restricted to these embodiment.
Embodiment 1
In Fig. 1, the pick-up unit of benzoyl peroxide is made of controller 1, low-light-level measurement device 2, kapillary 3, sample cell 4, tensimeter 5, pressure regulator 6, valve 7, gas cylinder 8, gland bonnet 9, computing machine 10 in the flour of present embodiment, tensimeter 5 is an embodiment of pressure indicator, and gas cylinder 8 is an embodiment of supercharging apparatus.Valve 7 is installed on the outlet conduit of gas cylinder 8, pressure regulator 6 is installed on the outlet conduit of valve 7, tensimeter 5 is installed on the pressure regulator 6, pressure regulator 6 links with gas cylinder 8 by the valve 7 that is installed on the pipeline, pressure regulator 6 is used for the compressed-air actuated pressure of gas cylinder 8 outputs is adjusted, and tensimeter 5 is used to indicate the pressure of pressure regulator 6 gas of adjusting.Pressure regulator 6 links by pipeline and sample cell 4, be stamped gland bonnet 9 on the sample cell 4, making sample cell 4 is an airtight container, can hold detected flour sample liquid in the sample cell 4, sample cell 4 links by kapillary 3 and low-light-level measurement device 2, the internal diameter of the kapillary 3 of present embodiment is 75 μ m, and kapillary 3 is to make with silica glass material.When the switch of opening gas cylinder 8 and valve 7, chemiluminescence reaction takes place in the flour sample liquid in the sample cell 4 in kapillary 3 flows to low-light-level measurement device 2 under compressed-air actuated effect.Low-light-level measurement device 2 is connected with computing machine 10, is connected with controller 1 by cable by cable.
In Fig. 2～5, the low-light-level measurement device 2 of present embodiment is to be connected by low-light-level measurement device housing 2-1, left end cap 2-2, power-line terminal 2-3, photomultiplier 2-4, chemiluminescence reaction pond 2-5, feed tube 2-6, feed liquor switch 2-7, right end cap 2-8, removal waste fluid pipe 2-9, removal waste fluid switch 2-10, signal output wiring terminal 2-11 to constitute, and photomultiplier 2-4 is an embodiment of photoelectric sensor.Left end at low-light-level measurement device housing 2-1 has left end cap 2-2, right-hand member by thread connection right end cap 2-8 to be arranged by thread connection, power-line terminal 2-3 and signal output wiring terminal 2-11 are installed on left end cap 2-2, the left side is equipped with photomultiplier 2-4 in low-light-level measurement device housing 2-1, and power-line terminal 2-3 is connected with photomultiplier 2-4 by lead with signal output wiring terminal 2-11.The right side is equipped with chemiluminescence reaction pond 2-5 in low-light-level measurement device housing 2-1, the chemiluminescence reaction pond 2-5 of present embodiment and removal waste fluid pipe 2-9 are connected as a single entity, removal waste fluid pipe 2-9 is arranged on the bottom face of chemiluminescence reaction pond 2-5, with link in the 2-5 of chemiluminescence reaction pond, the xsect of chemiluminescence reaction pond 2-5 is a rectangle, chemiluminescence reaction pond 2-5 and removal waste fluid pipe 2-9 make with quartzy transparent glass material, can hold chemical illuminating reagent in the 2-5 of chemiluminescence reaction pond, the chemical illuminating reagent of present embodiment is a luminol solution, removal waste fluid pipe 2-9 is interspersed with outside the low-light-level measurement device housing 2-1 from the bottom of low-light-level measurement device housing 2-1, removal waste fluid switch 2-10 is installed on removal waste fluid pipe 2-9, removal waste fluid switch 2-10 and removal waste fluid pipe 2-9 link, and chemical reacted waste liquid can be outside waste liquid switch 2-10 discharges low-light-level measurement device housing 2-1 in the 2-5 of chemiluminescence reaction pond.Top at low-light-level measurement device housing 2-1 is equipped with feed tube 2-6, feed tube 2-6 is interspersed with outside the low-light-level measurement device housing 2-1, the following top that is positioned at chemiluminescence reaction pond 2-5 that corrects of feed tube 2-6, feed liquor switch 2-7 is installed on the feed tube 2-6, feed liquor switch 2-7 and feed tube 2-6 link, when in the 2-5 of chemiluminescence reaction pond, adding chemical illuminating reagent, can add from feed liquor switch 2-7.On low-light-level measurement device housing 2-1 top kapillary 3 is installed, kapillary 3 is interspersed with outside the low-light-level measurement device housing 2-1, one end of kapillary 3 is inserted in the detected flour sample liquid in the sample cell 4, the other end is positioned at the top of chemiluminescence reaction pond 2-5, the height of chemical illuminating reagent liquid level is 3～4mm in the 2-5 of chemiluminescence reaction pond, open gas cylinder 8 and valve 7, detected flour sample liquid in the sample cell 4 is in kapillary 3 splashes into chemiluminescence reaction pond 2-5, every interval was dripped 1 in 20 seconds, and detected flour sample drop is gone in the 2-5 of chemiluminescence reaction pond and the luminol solution generation chemiluminescence reaction in the 2-5 of chemiluminescence reaction pond.Power-line terminal 2-3 is connected with controller 1 by cable, and controller 1 is used to control the power supply of photomultiplier 2-4.Signal output wiring terminal 2-11 is connected with computing machine 10 by cable.Photomultiplier 2-4 will receive chemiluminescence reaction is sent in the 2-5 of chemiluminescence reaction pond light signal and convert electric signal to and output to computing machine 10, the electric signal of 10 pairs of low-light-level measurement devices of computing machine, 2 outputs carries out data processing, demonstrates the content of benzoyl peroxide in the flour.
It is as follows to adopt pick-up unit of the present invention to detect in the flour benzoyl peroxide detection method:
(1) 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution preparation
Compound method is mixed with 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution routinely.
(2) luminol luminescence reagent preparation
Take by weighing 9 Crewe minots and 4 gram NaOH, pour in 1 liter of brown volumetric flask, add the 500mL redistilled water earlier, after treating to dissolve fully, vibration adds redistilled water again to scale mark, and making concentration is 5.0 * 10
-2The luminous stock solution of the luminol of mol/L is put the black out place, week back use.
With 5 milliliters of transfer pipets, pipette 5 milliliters of luminol stock solutions in 25 milliliters of volumetric flasks, add the NaHCO of 0.1mol/L
3-NaOH buffer solution is to scale mark, and making concentration is 1.0 * 10
-2The luminol luminescence reagent of mol/L.
(3) benzoyl peroxide standard solution preparation
Take by weighing the dry benzoyl peroxide 25mg that crosses, add in the 25mL volumetric flask, be settled to scale mark with absolute ethyl alcohol, being prepared into concentration is the standard stock solution of the benzoyl peroxide of 1mg/mL, places in the refrigerator and preserves.
With standard stock solution absolute ethyl alcohol stepwise dilution: the standard stock solution of getting 5mL concentration and be 1mg/mL adds in the 50mL volumetric flask, is settled to scale mark with absolute ethyl alcohol, 1.0 * 10
-4G/mL benzoyl peroxide titer; Getting 5mL concentration is 1.0 * 10
-4The titer of g/mL adds in the 50mL volumetric flask, is settled to scale mark with absolute ethyl alcohol, gets 1.0 * 10
-5G/mL benzoyl peroxide titer.Using the same method is settled to scale mark with absolute ethyl alcohol step by step, gets 1.0 * 10
-6G/mL, 1.0 * 10
-7G/mL, 1.0 * 10
-8The benzoyl peroxide titer of g/mL is used for the production standard curve.
(4) detected sample liquid preparation
Take by weighing commercially available flour 0.1g, move in the centrifuge tube, add the 5mL absolute ethyl alcohol, mixing and stirring, placed 10 minutes, and on hydro-extractor centrifugal 5 minutes, filtered with the rotating speed of 4000r/min, filter residue extracts 2 times with identical method, is settled to 25mL with absolute ethyl alcohol behind the merging filtrate, shakes up.
(5) making of typical curve
In 8 25mL volumetric flasks, measure 1.5mL, 2mL, 2.5mL, 5.0mL, 10mL, 15mL, 20mL, 25mL 1 * 10 with transfer pipet respectively
-8The benzoyl peroxide titer of g/mL is settled to scale mark with absolute ethyl alcohol, and being mixed with concentration is 6 * 10
-10G/mL, 8 * 10
-10G/mL, 1 * 10
-9G/mL, 2 * 10
-9G/mL, 4 * 10
-9G/mL, 6 * 10
-9G/mL, 8 * 10
-9G/mL, 1 * 10
-8The benzoyl peroxide titer of g/mL.Again in 10 25mL volumetric flasks, measure 1 * 10 of 0.5mL, 1.0mL, 1.5mL, 2mL, 2.5mL, 5.0mL, 10mL, 15mL, 20mL, 25mL with transfer pipet respectively
-6G/mL benzoyl peroxide titer is settled to scale mark with absolute ethyl alcohol, and being mixed with concentration is 2 * 10
-8G/mL, 4 * 10
-8G/mL, 6 * 10
-8G/mL, 8 * 10
-8G/mL, 1 * 10
-7G/mL, 2 * 10
-7G/mL, 4 * 10
-7G/mL, 6 * 10
-7G/mL, 8 * 10
-7G/mL, 1 * 10
-6The benzoyl peroxide titer of g/mL.Open the feed liquor switch 2-7 of low-light-level measurement device 2 upper ends, add 2mL luminol luminescence reagent in the 2-5 of chemiluminescence reaction pond.Getting 1～3mL benzoyl peroxide standard solution with the little centrifuge tube of tygon places in the sample cell 4, the sample introduction end of kapillary 3 inserts in the benzoyl peroxide standard solution, upper end cover top cover labyrinth 9 at sample cell 4, open the switch and the valve 7 of gas cylinder 8, regulate pressure regulator 6, the gas outlet pressure that makes pressure regulator 6 is 4kpa, benzoyl peroxide standard solution in the sample cell 4 carries out chemical reaction with the luminol luminescence reagent in kapillary 3 splashes into the chemiluminescence reaction pond 2-5 of low-light-level measurement device 2, regulating photomultiplier 2-4 negative high voltage is 800V, gain is 1, measure the values of chemiluminescence of each solution, concentration with the benzoyl peroxide standard solution is horizontal ordinate, chemiluminescence intensity is an ordinate relatively, uses computing machine 10 drawing standard curves, and draws the equation of linear regression of typical curve:
I
cl＝4.65(×10
9g/mL)C+8.28
Correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration (g/mL) of benzoyl peroxide, and detecting of benzoyl peroxide is limited to 1.4 * 10
-10G/mL.
(6) detection of benzoyl peroxide
Open the feed liquor switch 2-7 of low-light-level measurement device 2 upper ends, add 2mL luminol luminescence reagent in the 2-5 of chemiluminescence reaction pond.Getting the detected flour sample solution of 1～3mL with the little centrifuge tube of tygon places in the sample cell 4, the sample introduction end of kapillary 3 inserts in the sample solution, upper end cover top cover labyrinth 9 at sample cell 4, open the switch and the valve 7 of gas cylinder 8, regulate pressure regulator 6, making the gas outlet pressure of pressure regulator 6 is 4kpa, makes the sample solution in the sample cell 4 carry out chemical reaction with the luminol luminescence reagent in kapillary 3 splashes into the chemiluminescence reaction pond 2-5 of low-light-level measurement device 2, and its chemical equation is:
The negative high voltage of regulating photomultiplier 2-4 is 800v, gain is 1, photomultiplier 2-4 converts the light signal that receives to electric signal and outputs to computing machine 10, the electric signal of 10 pairs of inputs of computing machine carries out data processing, the chemiluminescent intensity level that middle per sample benzoyl peroxide oxidation luminol produces, find the concentration of benzoyl peroxide the flour sample solution from typical curve, perhaps press equation of linear regression:
I
cl＝4.65C(×10
9g/mL)+8.28
(correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration of benzoyl peroxide.)
The content that calculates benzoyl peroxide in the flour is 2.5 * 10
8C, unit are mg/Kg.
Embodiment 2
In the present embodiment, the internal diameter of the kapillary 3 of pick-up unit of the present invention is 50 μ m, chemiluminescence reaction pond 2-5 makes with quartzy transparent glass material, and the connecting relation of other parts and parts is identical with embodiment 1, and the detection method of present embodiment is identical with embodiment 1.
In the present embodiment, the internal diameter of the kapillary 3 of pick-up unit of the present invention is 100 μ m, chemiluminescence reaction pond 2-5 makes with quartzy transparent glass material, and the connecting relation of other parts and parts is identical with embodiment 1, and the detection method of present embodiment is identical with embodiment 1.
Embodiment 4
In above embodiment 1～3, chemiluminescence reaction pond 2-5 makes with transparent pmma material, and the connecting relation of other parts and parts is identical with respective embodiments, and the detection method of present embodiment is identical with embodiment 1.
In order to verify the beneficial effect of pick-up unit of the present invention and detection method thereof, the inventor adopts the embodiment of the invention 1 pick-up unit and detection method thereof that the content of benzoyl peroxide in benzoyl peroxide and the commercially available flour is detected, and detection case is as follows:
1, interference experiment
Experimental apparatus: pick-up unit of the present invention.
Laboratory sample: benzoyl peroxide.
Experimental technique: detection method of the present invention.
Experimental result: the concentration of benzoyl peroxide is 5 * 10
-8During g/mL, 1000 times K
+, Mg
2+, Ca
2+, Zn
2+, PO
4 3-, NO
2 -, NH
4 +, starch, glucose, 100 times Cu
2+, Pb
2+, Cr
3+, S
2-, NO
3 -, SO
4 2-, VB
1, Vc, glutamic acid, proline, 10 times Fe
3+, Co
2+, Ni
2+, Cd
2+, leucine, VB
2Interference measurement not.
Experiment conclusion: the selectivity that detection method of the present invention is measured benzoyl peroxide is good.
2, the precision of detection method of the present invention experiment
Experimental apparatus: pick-up unit of the present invention.
Laboratory sample: benzoyl peroxide.
Experimental technique: detection method of the present invention.
Experimental result: under experiment condition, to 2.0 * 10
-8The relative standard deviation that the g/mL benzoyl peroxide carries out 11 parallel replications is 1.5%, and it measures collection of illustrative plates referring to Fig. 7.
Experiment conclusion: experimental result shows the favorable reproducibility of detection method of the present invention.
3, the range of linearity and detection limit experiment
Experimental apparatus: pick-up unit of the present invention.
Laboratory sample: benzoyl peroxide.
Experimental technique: detection method of the present invention.
Experimental result: under the condition of selecting, the concentration of benzoyl peroxide is 6.0 * 10
-10～1.0 * 10
-6Be good linear relationship with luminous intensity in the g/mL scope, its equation of linear regression is:
I
cl＝4:65C(×10
9g/mL)+8.28
R=0.9986, detecting of benzoyl peroxide is limited to 1.4 * 10
-10G/mL.
Experiment conclusion: detection method of the present invention measures that the range of linearity of benzoyl peroxide is wide, detection limit is low, highly sensitive.
4, the mensuration of flour sample and recovery experiment
Experimental apparatus: pick-up unit of the present invention.
Laboratory sample: commercially available flour.
Experimental technique: 6 flour samples are carried out the assay of benzoyl peroxide (BPO) and carry out recovery test by embodiment 1 detection method of the present invention.
Testing result: testing result sees Table 1.
The measurement result of benzoyl peroxide (n=6) in table 1 flour.
Sample BPO (mg/Kg) the BPO standard solution BPO standard solution recovery (%)
Addition (mg/Kg) amount of recording (mg/Kg)
1* 0.0 30.0 29.8 99.3
2 7.1 10.0 16.9 98.0
3 12.3 10.0 22.0 97.0
4 42.6 30.0 73.1 101.7
5 12.4 10.0 22.6 102.0
6 35.2 10.0 45.5 103.0
* measure after becoming flour by fresh wheat flour milling.
Detect conclusion: from the data of table 1 as can be known, the standard recovery that detection method of the present invention is measured benzoyl peroxide is 97%～103%.
Claims (6)
1, the pick-up unit of benzoyl peroxide in a kind of flour is characterized in that it comprises:
Compressed-air actuated gas cylinder [8] can be provided;
Be provided with the pressure regulator [6] of tensimeter [5];
Be arranged on valve [7] or switch on the pipeline that links between gas cylinder [8] and the pressure regulator [6];
The top is provided with the sample cell [4] that gland bonnet [9] can hold detected sample solution, and this sample cell [4] links by pipeline and pressure regulator [6];
The low-light-level measurement device [2] that links by kapillary [3] and sample cell [4], this low-light-level measurement device [2] comprising: low-light-level measurement device housing [2-1], left end cap [2-2], power-line terminal [2-3], photomultiplier [2-4], chemiluminescence reaction pond [2-5], feed tube [2-6], feed liquor switch [2-7], right end cap [2-8], removal waste fluid pipe [2-9], removal waste fluid switch [2-10], signal output wiring terminal [2-11], left end cap [2-2] is arranged on the left end of low-light-level measurement device housing [2-1], right end cap [2-8] is arranged on the right-hand member of low-light-level measurement device housing [2-1], chemiluminescence reaction pond [2-5] is arranged on the interior right side of low-light-level measurement device housing [2-1], photomultiplier [2-4] is arranged on left side in the low-light-level measurement device housing [2-1], the sample outlet end of kapillary [3] penetrates and is arranged on top, chemiluminescence reaction pond [2-5] in the low-light-level measurement device housing [2-1], feed tube [2-6] is arranged on chemiluminescence reaction pond [2-5] top and passes low-light-level measurement device housing [2-1] and link with the feed liquor switch [2-7] that is installed on the feed tube [2-6], removal waste fluid pipe [2-9] and chemiluminescence reaction pond [2-5] link and pass low-light-level measurement device housing [2-1] and link with the removal waste fluid switch [2-10] that is installed on the removal waste fluid pipe [2-9], and the power-line terminal [2-3] that is arranged on the left end cap [2-2] is connected with photomultiplier [2-4] by lead with signal output wiring terminal [2-11];
It comprises the controller [1] that is used to control low-light-level measurement device [2], and this controller [1] is connected with low-light-level measurement device [2] by cable or wire;
It also comprises the computing machine [10] that is used to carry out data processing, and this computing machine [10] is connected with signal output wiring terminal [2-11] by cable.
2, according to the pick-up unit of benzoyl peroxide in the described flour of claim 1, it is characterized in that: said chemiluminescence reaction pond [2-5] is to make with the organic or inorganic transparent material.
3, according to the pick-up unit of benzoyl peroxide in claim 1 or the 2 described flour, it is characterized in that: the horizontal section in said chemiluminescence reaction pond [2-5] is a rectangle.
4, according to the pick-up unit of benzoyl peroxide in the described flour of claim 1, it is characterized in that: the internal diameter of said kapillary [3] is 50 μ m or 75 μ m or 100 μ m.
5, according to the pick-up unit of benzoyl peroxide in claim 1 or the 4 described flour, it is characterized in that: said kapillary [3] is to make with silica glass material.
6, a kind of detection method of using the device described in the claim 1 to carry out benzoyl peroxide in the flour is characterized in that it comprises the steps:
(1) 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution preparation
Compound method is mixed with 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution routinely;
(2) luminescence reagent preparation
The luminol or derivatives thereof is prepared into luminescence reagent according to a conventional method with 0.1mol/L sodium bicarbonate-sodium hydroxide buffer solution;
(3) preparation of benzoyl peroxide standard solution
Take by weighing benzoyl peroxide 25mg, add in the 25mL volumetric flask, be settled to scale mark with absolute ethyl alcohol, being prepared into concentration is the standard stock solution of the benzoyl peroxide of 1mg/mL, places in the refrigerator and preserves, and uses the absolute ethyl alcohol stepwise dilution during use;
(4) detected sample liquid preparation
Take by weighing commercially available flour 0.1g, move in the centrifuge tube, add the 5mL absolute ethyl alcohol, mixing and stirring, placed 10 minutes, and on hydro-extractor centrifugal 5 minutes, filtered with the rotating speed of 4000r/min, filter residue extracts 2 times with identical method, is settled to 25mL with absolute ethyl alcohol behind the merging filtrate, shakes up;
(5) making of typical curve
Standard stock solution with absolute ethyl alcohol stepwise dilution benzoyl peroxide is mixed with concentration 6.0 * 10
-10～1.0 * 10
-6Benzoyl peroxide standard solution in the g/mL scope, to be settled to scale mark, open the feed liquor switch [2-7] of low-light-level measurement device [2] upper end, add 1～3mL luminescence reagent in chemiluminescence reaction pond [2-5], getting 1～3mL benzoyl peroxide standard solution with the little centrifuge tube of tygon places in the sample cell [4], the sample introduction end of kapillary [3] inserts in the sample solution, upper end cover top cover labyrinth [9] at sample cell [4], open the switch and the valve [7] of gas cylinder [8], the gas outlet pressure of regulating pressure regulator [6] is 4kpa, benzoyl peroxide standard solution in the sample cell [4] in kapillary [3] splashes into the chemiluminescence reaction pond [2-5] of low-light-level measurement device [2] and luminescence reagent carry out chemical reaction, regulating photomultiplier [2-4] negative high voltage is 800v, gain is 1, measuring the values of chemiluminescence of each solution, is horizontal ordinate with the concentration of benzoyl peroxide standard solution, and chemiluminescence intensity is an ordinate relatively, with computing machine [10] drawing standard curve, its equation of linear regression is:
I
cl＝4.65(×10
9g/mL)C+8.28
Correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration of benzoyl peroxide, and unit is g/mL, and detecting of benzoyl peroxide is limited to 1.4 * 10
-10G/mL;
(6) detection of benzoyl peroxide
Open the feed liquor switch [2-7] of low-light-level measurement device [2] upper end, add 1～3mL luminescence reagent in chemiluminescence reaction pond [2-5], getting the detected flour sample solution of 1～3mL with the little centrifuge tube of tygon places in the sample cell [4], the sample introduction end of kapillary [3] inserts in the sample solution, upper end cover top cover labyrinth [9] at sample cell [4], open the switch and the valve [7] of gas cylinder [8], the gas outlet pressure of regulating pressure regulator [6] is 4kpa, sample solution in the sample cell [4] in kapillary [3] splashes into the chemiluminescence reaction pond [2-5] of low-light-level measurement device [2] and luminescence reagent carry out chemical reaction, the negative high voltage of regulating photomultiplier [2-4] is 800v, gain is 1, and computing machine is pressed equation of linear regression:
I
cl＝4.65(×10
9g/mL)C+8.28
Correlation coefficient r=0.9986, I in the formula
ClBe chemiluminescence intensity, C is the concentration of benzoyl peroxide, and the content that computing machine [10] calculates benzoyl peroxide in the flour is 2.5 * 10
8C, unit are mg/Kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03114697XA CN1195218C (en) | 2003-04-28 | 2003-04-28 | Detection device of benzoperoxide in flour and detection method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03114697XA CN1195218C (en) | 2003-04-28 | 2003-04-28 | Detection device of benzoperoxide in flour and detection method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1444034A CN1444034A (en) | 2003-09-24 |
| CN1195218C true CN1195218C (en) | 2005-03-30 |
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ID=27814819
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB03114697XA Expired - Fee Related CN1195218C (en) | 2003-04-28 | 2003-04-28 | Detection device of benzoperoxide in flour and detection method |
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| CN (1) | CN1195218C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102004094B (en) * | 2010-09-14 | 2012-03-14 | 陕西师范大学 | Method for detecting content of benzoyl peroxide in flour |
| CN102207466B (en) * | 2011-04-06 | 2013-04-24 | 江苏财经职业技术学院 | Rapid test kit for benzoyl peroxide banned additive in flour |
| CN102353667B (en) * | 2011-07-05 | 2013-01-09 | 邢台市产品质量监督检验所 | Method for detecting content of benzoyl peroxide in flour |
| CN103792233B (en) * | 2014-03-04 | 2015-11-25 | 河南工业大学 | Pick-up unit and detection method while potassium bromate and benzoyl peroxide in wheat flour |
| CN105301120A (en) * | 2014-07-24 | 2016-02-03 | 王勇 | Detecting method of benzoyl peroxide in wheat flour |
| CN106018386B (en) * | 2016-04-20 | 2019-04-16 | 浙江大茗堂生物科技有限公司 | The analysis method of oxidation resistance in a kind of tealeaves or tea product |
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2003
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