CN101344483A - Method for detecting lead content in milk and milk product - Google Patents
Method for detecting lead content in milk and milk product Download PDFInfo
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- CN101344483A CN101344483A CNA2008101322492A CN200810132249A CN101344483A CN 101344483 A CN101344483 A CN 101344483A CN A2008101322492 A CNA2008101322492 A CN A2008101322492A CN 200810132249 A CN200810132249 A CN 200810132249A CN 101344483 A CN101344483 A CN 101344483A
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Abstract
The invention relates to a method used for detecting the content of a heavy metal plumbum in milk and milk products and comprises the following steps: (1) a specification curve is plotted; (2) a sample is prepared, and the machine detection with a prepared reducing agent and carrying fluid is implemented, thus obtaining a detected result; (3) the detected result obtained from step (2) is contrasted with the specification curve, thus obtaining the plumbum content in the sample; and (4) an atomic fluorophotometer is taken as a detecting instrument in above steps. The method optimizes the working conditions and the experimental conditions of the atomic fluorophotometer, adds red potassium prussiate into the reducing agent under a chosen optimal measuring condition, and controls the acidity of a reacting solution. The method has low detection limit, high sensitivity and low instrument price, and is applicable to analyzing the plumbum content in milk and milk products.
Description
Technical field
The present invention relates to a kind of detection method, particularly a kind of method that detects content of heavy metal lead in breast and the dairy products.Belong to the technical field that chemical analysis detects.
Background technology
Lead is one of extremely strong heavy metal of known toxicity maximum, cumulative bad.When lead is accumulated in human body for a long time, meeting serious harm nerve, hemopoietic system and digestive system, especially serious to baby's intelligence and body development influence.Be listed in the important element of Food Hygiene Surveillance.The assay method of trace lead is a lot of at present, and prussiate Generation-Atomic Fluorescence Spectrometry sounding lead is a kind of faster new analytical technology of developed recently.
After hydride-atomic fluorescence spectrometry added sample acid and clears up, in acid medium, lead in the sample and potassium borohydride reaction generated plumbous hydride.With the argon gas is carrier gas, hydride is imported atomization in the electric heating quartz atomizer, under plumbous hollow cathode light irradiation, the ground state lead atom is excited to high-energy state, deactivating when getting back to ground state, launch the fluorescence of characteristic wavelength, its fluorescence intensity is directly proportional with lead content, carries out quantitatively according to standard series.The potassium ferricyanide directly adds in the sample solution in the method for existing AFS DETERMINATION Ruzhong lead, poor stability, and precision is low.
Summary of the invention
The purpose of this invention is to provide a kind of method that detects content of heavy metal lead in breast and the dairy products, its good stability, precision is higher.
The invention provides a kind of method that detects content of heavy metal lead in breast and the dairy products, comprise the steps:
1) drawing standard curve: prepare the plumbous standard solution of a plurality of variable concentrations, and it is detected respectively,, draw the typical curve between lead content and the testing result according to measured data;
2) the preparation sample also with machine testing on reductive agent for preparing and the current-carrying liquid, obtains testing result;
3) with step 2) in testing result and described typical curve comparison, promptly obtain content plumbous in the sample;
4) employed detecting instrument is an atomic fluorescence spectrophotometer in the above-mentioned steps.
Preferably, above-mentioned steps 1) in plumbous concentration of standard solution be 0.0,2.0,4.0,6.0,8.0,10.0ng/mL.The compound method of above-mentioned standard solution is: add plumbous standard application liquid (100ng/mL) 0.0,0.5,1.0,1.5,2.0,2.5mL, after a small amount of pure water dilution, each adds 0.5mL hydrochloric acid and 0.5mL 10g/L oxalic acid solution, accurately is settled to 25mL with pure water, shake up, place 30min.
Preferred, step 2) preparation method of sample may further comprise the steps in:
A) take by weighing sample in the micro-wave digestion pipe, add nitric acid, after the micro-wave digestion stove is cleared up fully, add water, on electric hot plate, catch up with acid; Catch up with sour 3-4 time.
B) catch up with acid with pure water sample to be washed in the volumetric flask back fully, constant volume shakes up;
C) react back waste liquid acidity per sample,, place 30min with pure water diluted sample liquid;
Above-mentioned steps c) available pure water is diluted to suitable concn to test liquid and makes reacted waste liquor PH value be controlled at 8-9 in.
Among the present invention, step 2) reductive agent in preferably is grouped into by following one-tenth: NaOH (or potassium hydroxide) 5g/L, potassium borohydride 20-40g/L, potassium ferricyanide 15-25g/L, preferred, the concentration of potassium borohydride is 20g/L, and the concentration of the potassium ferricyanide is 15g/L.Its preparation method is: first dissolved hydrogen sodium oxide molybdena, dissolve potassium borohydride, behind the last dissolved iron potassium cyanide, with pure water dissolving and constant volume again.
Among the present invention, step 2) the current-carrying liquid in is 2% hydrochloric acid (v/v) preferably.
Atomic fluorescence spectrophotometer detected parameters among the present invention is preferably: when the stove height is 6mm, and negative high voltage 220V-230V, lamp current 60-65mA, carrier gas and shielding gas are argon gas, flow is respectively 400mL/min and 1000mL/min.
The method that detects content of heavy metal lead in breast and the dairy products of the present invention joins the potassium ferricyanide in the reductive agent, the acidity of control reaction solution, detect and be limited to 0.1106 μ g/L, the recovery is that 95%-105%, relative standard deviation are 0.6%, be directed to existing method, its precision obviously improves.And, highly sensitive, instrument is cheap under the detected parameters of the present invention, be suitable for the content of lead in macromethod breast and the dairy products.
Description of drawings
Fig. 1 shows is the high relation with fluorescence intensity of stove in one embodiment of the present of invention;
Fig. 2 shows is the relation of potassium ferricyanide concentration and fluorescence intensity in one embodiment of the present of invention;
Fig. 3 shows is the relation of potassium borohydride concentration and fluorescence intensity in one embodiment of the present of invention;
Fig. 4 shows is the relation of hydrochloric acid addition and fluorescence intensity in one embodiment of the present of invention;
What Fig. 5 showed is the relation of one embodiment of the present of invention mesoxalic acid addition and fluorescence intensity;
What Fig. 6 showed is plumbous typical curve synoptic diagram in one embodiment of the present of invention.
Specific embodiments
Below in conjunction with specific embodiments method of the present invention is done more detailed description.It will be appreciated by those skilled in the art that following embodiment all is used for the present invention's scope required for protection is carried out the description of exemplary, summarize the relative scope of each parameter of the present invention, thereby it can not be interpreted as a kind of concrete restriction of the present invention with this.
The selection of embodiment 1 detected parameters and drawing standard curve
1. experimental procedure
1.1 instrument and reagent
AFS-2202E type two pass atomic fluorescence spectrophotometer (Haiguang Instrument Corp, Beijing)
Micro-wave digestion stove (U.S. CE M, MARS XPRESS)
Electric hot plate
Plumbous standard reserving solution: 1000 μ g/mL, national standard material center
Plumbous standard application liquid: 100ng/mL accurately draws plumbous standard reserving solution, and stepwise dilution is to 100ng/mL.
Oxalic acid solution (10g/L): take by weighing 1.0g oxalic acid, add the pure water dissolving and be settled to 100mL, mixing.
Reductive agent: by NaOH 1 gram, potassium borohydride 4 grams and the potassium ferricyanide 3 grams are formed.Elder generation's dissolved hydrogen sodium oxide molybdena dissolves potassium borohydride again, and last dissolved iron potassium cyanide is with the pure water dissolving and be settled to 200mL, matching while using.Above-mentioned NaOH can be replaced by potassium hydroxide.
Hydrochloric acid (2%): draw 10mL hydrochloric acid, be settled to 500mL with pure water.
Nitric acid, hydrochloric acid: top grade is pure.
1.2 instrument condition
Lamp current: 60mA; Photomultiplier negative high voltage: 220V;
Atomizer height: 6mm;
Carrier gas (argon gas) flow: 400mL/min;
Shielding gas (argon gas) flow: 1000mL/min;
Reading duration: 10s;
Time delay: 1.0s;
Measuring method: calibration curve method;
Read mode: peak area;
Reductive agent: NaOH 1 gram, potassium borohydride 4 grams, the potassium ferricyanide 3 grams, first dissolved hydrogen sodium oxide molybdena dissolves potassium borohydride again, behind the last dissolved iron potassium cyanide, with the pure water dissolving and be settled to 200mL, matching while using;
Screening agent: 10g/L oxalic acid;
Current-carrying liquid: 2% hydrochloric acid.
1.3 the drafting of standard working curve
Get 6 in 25ml volumetric flask, add plumbous standard application liquid 0.0,0.5,1.0,1.5,2.0,2.5mL (respectively being equivalent to lead concentration 0.0,2.0,4.0,6.0,8.0,10.0ng/mL) successively, after a small amount of pure water dilution, each adds 0.5mL hydrochloric acid and 0.5mL 10g/L oxalic acid solution, accurately be settled to 25mL with pure water, shake up.Detect after placing 30min.
1.4 sample preparation
Take by weighing 0.5-1.0 gram breast or milk powder sample, place the micro-wave digestion pipe, add 10 milliliters of nitric acid, after the micro-wave digestion stove is cleared up fully, add the 20mL pure water, on electric hot plate, catch up with acid 3 times.Wash in the 25mL volumetric flask with pure water, and accurately be settled to 25mL, shake up.Dilute with pure water according to reaction back waste liquid acidity, pH value is controlled at 8-9, approximately dilute 5 times, detect by above-mentioned condition of work behind the placement 30min.The micro-wave digestion condition sees Table 1.
Table 1 micro-wave digestion condition
2. the selection of testing conditions
2.1 the selection of Instrument working parameter experiment:
2.1.1 stove height: respectively with stove to a high-profile to 4,5,6,7,8mm surveys fluorescence intensity, atomizer increases, i.e. stove higher primary school, the fluorescence intensity increase serious interference can occur when too high, background noise is excessive, atomizer is low excessively, fluorescence intensity is low.What Fig. 1 showed is the experimental result curve of stove height and fluorescence intensity, and when the stove height was 6mm, instrumental sensitivity and stability were better.
2.1.2 negative high voltage: along with the increase of negative high voltage, the also corresponding increase of fluorescence intensity, but the also corresponding increase of noise.What Fig. 2 showed is the experimental result curve of potassium ferricyanide concentration and fluorescence intensity; Experiment showed, that selecting negative high voltage is 220V-230V, fluorescence intensity is comparatively stable.
2.1.3 lamp current: along with the enhancing of lamp current, fluorescence intensity increases, and lamp current is crossed instability when hanging down, and influences the serviceable life of lamp when too high.Experiment showed, that selection lamp current 60-65mA fluorescence intensity is better.
2.1.4 carrier gas (argon gas), shielding gas (argon gas) flow: carrier gas is excessive, is equivalent to the concentration of dilute sample, and fluorescence intensity is reduced.When carrier gas is too small, flame instability.Present embodiment selects carrier gas, shield gas flow amount to be respectively 400mL/min and 1000mL/min.
2.2 the selection of iron hydrofining concentration
The potassium ferricyanide is as matrix modifier, can reduce the interference that other metal causes, it by concentration relatively 0%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0% potassium ferricyanide solution, experimental result as shown in Figure 2, fluorescence intensity is stable when finding in the 1.5%-2.5% scope.It is 1.5% that present embodiment is selected to add potassium ferricyanide concentration.
2.3 the selection of potassium borohydride concentration
Found through experiments fluorescence intensity and increase with borane reducing agent hydrofining concentration, as shown in Figure 3, fluorescence intensity tends towards stability in the potassium borohydride concentration 2.0%-4.0% scope.It is 2% that present embodiment preferably adds potassium borohydride concentration.
2.4 the selection of acidity
Plumbous hydride reaction of formation condition requires very harsh to acidity, require the pH value scope of reaction back waste liquid to be controlled at about 8-9.Fluorescence intensity was stable when as shown in Figure 4, adding concentrated hydrochloric acid amount was 0.5-1.0mL in the 50mL system.Preferred adding hydrochloric acid content is 1.0mL.
2.5 the influence of screening agent oxalic acid addition
As shown in Figure 5, experiment shows, fluorescence intensity is stable during 10g/L oxalic acid addition 0.5-1.5mL in the 50mL system.Preferred oxalic acid addition is 1.0mL.
2.6 typical curve and linear range
Running parameter:
Instrument parameter: the stove height is 6mm, negative high voltage 220V-230V, and lamp current 60-65mA, carrier gas and shielding gas are argon gas, flow is respectively 400mL/min and 1000mL/min.
Standard solution is detected, the drawing standard working curve, as shown in Figure 6, related coefficient is 0.9996, regression equation is If=79.27*C+18.912.Record plumbous linear in the 0-100ng/mL scope through test.
2.7 minimum detectability
Measure program according to the detection limit that instrument is given, the fluorescence signal of METHOD FOR CONTINUOUS DETERMINATION standard blank solution and standard series calculates detecting of the method and is limited to 0.1106 μ g/L.
2.8 precision is investigated
By 11 duplicate measurements concentration of experimental technique is the plumbous standard solution of 10.00 μ g/L, and calculating relative standard deviation is 0.6%.
2.9 recovery of standard addition experiment
Adopt the mark-on recovery method, take by weighing the sample of known content, the plumbous standard solution that adds three kinds of variable concentrations is respectively done recovery experiment, and testing result sees Table 2.
Table 2 recovery experimental result
Under selected optimum determining condition, the method detects and is limited to 0.1106 μ g/L, the recovery is that 95%-105%, relative standard deviation are 0.6%.Show that method of the present invention is that a kind of detection limit is low, highly sensitive, instrument is cheap, be applicable to the method for analyzing lead content in breast and the dairy products.
By the present invention and 11 concentration of existing experimental technique duplicate measurements is the plumbous standard solution of 10.00 μ g/L, calculates its precision, and experimental result sees Table 3.
Simultaneously, be the plumbous standard solution of 10.00 μ g/L with existing 11 concentration of method duplicate measurements, calculate its precision, experimental result sees Table 4.
The step of existing method is as follows: accurately draw the plumbous standard application liquid of 5.00 milliliters of 100ng/mL in 50 milliliters of volumetric flasks, add 1.0mL hydrochloric acid (1+1), 1.0mL 10g/L oxalic acid solution, 2.0mL100g/L potassium ferricyanide solution, accurately be settled to 50mL with pure water, mixing is mixed with the plumbous standard solution of 10.00 μ g/L.With the reductive agent for preparing and 11 its fluorescence intensities of duplicate measurements of current-carrying liquid, instrument calculates precision automatically.
The detected parameters of existing method: stove height: 8mm, negative high voltage 323V, lamp current 75mA, carrier gas (argon gas) flow 800mL/min, shielding gas (argon gas) flow 1000mL/min, reductive agent: take by weighing the 5.0g sodium borohydride and be dissolved in 500 milliliters of 2g/L sodium hydroxide solutions, mixing, matching while using.
Table 3 method precision experimental result of the present invention
Table 4 has the method precision experimental result now
From above testing result as can be seen the inventive method than existing method good stability, precision height.This inventive method is controlled the acidity of reaction solution by the potassium ferricyanide is joined in the reductive agent, and effect is obvious.
Testing conditions adopts 1 preferred parameter of embodiment.
Experimental procedure:
1) take by weighing 0.5-1.0 gram sample, yaourt, plain chocolate add 10 milliliters of nitric acid in the micro-wave digestion pipe, add 20mL water and catch up with acid 3 times after the micro-wave digestion stove is cleared up fully on electric hot plate.
2) catch up with acid to wash in the 25mL volumetric flask with pure water and accurately be settled to 25mL in the back fully, shake up.
3) accurately draw the good sample liquid of 5.00 milliliters of above-mentioned constant volumes in the 25mL volumetric flask, add the 0.5mL10g/L oxalic acid solution, be settled to 25 milliliters, place 30min with pure water.At this moment, test liquid reaction back waste liquid pH value is in the 8-9 scope.
4) preparation of reductive agent: NaOH 1 gram, potassium borohydride 4 grams, the potassium ferricyanide 3 grams, first dissolved hydrogen sodium oxide molybdena dissolves potassium borohydride again, and last dissolved iron potassium cyanide is with the pure water dissolving and be settled to 200mL, matching while using.
5) preparation of current-carrying liquid: draw the 10mL concentrated hydrochloric acid, be settled to 500mL with pure water, mixing.
6) preparation of standard serial solution: get 6 in 25ml volumetric flask, add plumbous standard application liquid 0.0,0.5,1.0,1.5,2.0,2.5ml (respectively being equivalent to lead concentration 0.0,2.0,4.0,6.0,8.0,10.0, ng/mL) successively, after a small amount of pure water dilution, each adds 0.5mL hydrochloric acid and 0.5mL 10g/L oxalic acid solution, accurately is settled to 25mL, shakes up with pure water.Place 30min.
7) with machine testing on reductive agent for preparing and the current-carrying liquid.With testing result and typical curve contrast, obtain content plumbous in each sample.
Testing result is as shown in table 5.
Table 5 detects the result of breast and dairy products lead content
The method that detects content of heavy metal lead in breast and the dairy products of the present invention joins the potassium ferricyanide in the reductive agent, the acidity of control reaction solution, detect and be limited to 0.1106 μ g/L, the recovery is that 95%-105%, relative standard deviation are 0.6%, than existing method, its precision obviously improves.And, highly sensitive, instrument is cheap under the detected parameters of the present invention, be suitable for the content of lead in macromethod breast and the dairy products.
Claims (10)
1. a method that detects content of heavy metal lead in breast and the dairy products comprises the steps:
1) drawing standard curve: prepare the plumbous standard solution of a plurality of variable concentrations, and it is detected respectively,, draw the typical curve between lead content and the testing result according to measured data;
2) the preparation sample also with machine testing on reductive agent for preparing and the current-carrying liquid, obtains testing result;
3) with step 2) in testing result and described typical curve comparison, promptly obtain content plumbous in the sample;
4) employed detecting instrument is an atomic fluorescence spectrophotometer in the above-mentioned steps.
2. the method for claim 1 is characterized in that, the plumbous concentration of standard solution in the described step 1) is 0.0,2.0,4.0,6.0,8.0,10.0ng/mL.
3. method as claimed in claim 2, it is characterized in that, the compound method of the plumbous standard solution of described usefulness is: add plumbous standard application liquid (100ng/mL) 0.0,0.5,1.0,1.5,2.0,2.5mL, after a small amount of pure water dilution, each adds 0.5mL hydrochloric acid and 0.5mL 10g/L oxalic acid solution, accurately be settled to 25mL with pure water, shake up, place 30min.
4. the method for claim 1 is characterized in that, described step 2) described in the preparation method of sample may further comprise the steps:
A) take by weighing sample in the micro-wave digestion pipe, add nitric acid, after the micro-wave digestion stove is cleared up fully, add water, on electric hot plate, catch up with acid;
B) catch up with acid with pure water sample to be washed in the volumetric flask back fully, constant volume shakes up;
C) react back waste liquid acidity per sample,, place 30min with pure water dilute sample solution;
5. method as claimed in claim 4 is characterized in that, describedly catches up with acid to carry out 3-4 time.
6. the method that detects content of heavy metal lead in breast and the dairy products as claimed in claim 5 is characterized in that the reacted waste liquor PH value of test liquid is controlled at 8-9 in the described step c).
7. method as claimed in claim 6 is characterized in that, with pure water test liquid is diluted five times in the described step c).
8. the method that detects content of heavy metal lead in breast and the dairy products as claimed in claim 1, it is characterized in that described step 2) in reductive agent be grouped into by following one-tenth: NaOH (or potassium hydroxide) 5g/L, potassium borohydride 20-40g/L, potassium ferricyanide 15-25g/L, its preparation method is: first dissolved hydrogen sodium oxide molybdena, dissolve potassium borohydride again, behind the last dissolved iron potassium cyanide, with pure water dissolving and constant volume.
9. the method for claim 1 is characterized in that, described step 2) in current-carrying liquid be 2% hydrochloric acid (v/v).
10. the method for claim 1 is characterized in that, described atomic fluorescence spectrophotometer detected parameters is: when the stove height is 6mm, negative high voltage 220V-230V, lamp current 60-65mA, carrier gas and shielding gas are argon gas, flow is respectively 400mL/min and 1000mL/min.
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| CN108931407A (en) * | 2018-04-12 | 2018-12-04 | 江西省兽药饲料监察所 | Determining heavy metals pre-treating method in a kind of pig manure |
| CN109374884A (en) * | 2018-12-24 | 2019-02-22 | 四川沃文特生物技术有限公司 | A kind of PCT concentration detection kit and preparation method thereof |
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