CN112816429A - Method for measuring lead content in food - Google Patents
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- CN112816429A CN112816429A CN202011641532.5A CN202011641532A CN112816429A CN 112816429 A CN112816429 A CN 112816429A CN 202011641532 A CN202011641532 A CN 202011641532A CN 112816429 A CN112816429 A CN 112816429A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a method for measuring lead content in food, which comprises the steps of preparing a reagent and preparing the reagent; preparing a standard solution and preparing instruments and equipment; preparing a sample; carrying out pretreatment on the sample by adopting wet digestion, microwave digestion and pressure tank digestion respectively; and (4) preparing a standard curve, measuring the sample solution, digesting the sample, atomizing the sample by a graphite furnace, and measuring the absorbance at 283.3 nm. The absorbance value of the lead in a certain concentration range is in direct proportion to the lead content, and the absorbance value is compared and quantified with a standard series, so that the lead content in the food can be well measured. The invention solves the problem that the content of lead in food is harmful to human bodies greatly, and a better determination method for determining the content of lead in food does not exist at present.
Description
Technical Field
The invention relates to the technical field of lead content determination, in particular to a method for determining the lead content in food.
Background
Food refers to various finished products and raw materials for people to eat or drink and the products which are food and traditional Chinese medicinal materials according to the tradition, but do not include the products for treating. The definition for food products is: substances which can be consumed or drunk by humans, including processed foods, semi-finished products and unprocessed foods, excluding tobacco or substances used only as medicines.
Lead is a metal chemical element and is the most atomic, non-radioactive element. The metal lead is a face-centered cubic crystal, the content of lead in food is harmful to human bodies, and a better determination method for determining the content of lead in food does not exist at present, so that a determination method for the content of lead in food is designed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for measuring the content of lead in food, which solves the problem that the content of lead in food is more harmful to human bodies, and no better measuring method for measuring the content of lead in food exists at present.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for measuring the lead content in food comprises the following steps,
(1) preparing a reagent and preparing the reagent;
(2) preparing a standard solution and preparing instruments and equipment;
(3) preparing a sample;
(4) carrying out pretreatment on the sample by adopting wet digestion, microwave digestion and pressure tank digestion respectively;
(5) a standard curve is prepared, and the sample solution is measured.
In the method for measuring the lead content in the food, in the step (1), the prepared reagent is nitric acid (HNO)3)、Perchloric acid (HClO)4) Ammonium dihydrogen phosphate (NH4H2PO4) and palladium nitrate [ Pd (NO3)2 ]]Then, the reagent is prepared,
(A1) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 950mL of water, and uniformly mixing;
(A2) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 450mL of water, and uniformly mixing;
(A3) and (3) weighing 0.02g of palladium nitrate, adding a small amount of nitric acid solution to dissolve the palladium nitrate, then adding 2g of ammonium dihydrogen phosphate, dissolving, metering the volume to 100mL by using nitric acid solution, and uniformly mixing.
In the method for measuring the lead content in the food, in the step (2), the preparation of the standard solution comprises,
(B1) lead standard stock solution: accurately weighing 1.5985-1.6013g of lead nitrate, dissolving the lead nitrate by using a small amount of nitric acid solution, transferring the lead nitrate into a 1000mL volumetric flask, adding water to the scale, and uniformly mixing;
(B2) lead standard intermediate solution: accurately sucking 1.00mL of lead standard stock solution into a 1000mL volumetric flask, adding a nitric acid solution to a scale, and uniformly mixing;
(B3) and (3) respectively sucking 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL and 4.00mL of the lead standard intermediate solution into a 100mL volumetric flask, adding a nitric acid solution to the scales, and uniformly mixing, wherein the mass concentrations of the lead standard intermediate solution are respectively 0 mug/L, 5.00 mug/L, 10.0 mug/L, 20.0 mug/L, 30.0 mug/L and 40.0 mug/L.
In the step (2), the apparatus and equipment include an atomic absorption spectrometer, an analytical balance, an adjustable electric furnace, an adjustable electric hot plate, a microwave digestion system, a constant temperature drying oven and a pressure digestion tank.
In the method for measuring the content of lead in food, in the step (3), the samples of vegetables, fruits, fishes and meats are washed with water, dried, and the edible parts are prepared into homogenate and stored in a plastic bottle.
In the method for measuring the lead content in the food, in the step (4), the wet digestion is as follows: weighing 0.2-3 g of solid sample or accurately transferring 0.500-5.00 mL of liquid sample into a graduated digestion tube, adding 10mL of nitric acid and 0.5mL of perchloric acid, digesting on an adjustable electric heating furnace, adding a small amount of nitric acid if the digestion solution is tan, digesting until white smoke appears, taking out the digestion tube, cooling, adding water to a constant volume of 10mL, uniformly mixing for later use, and simultaneously performing a reagent blank test;
the microwave digestion: weighing 0.2-0.8 g of solid sample or accurately transferring 0.500-3.00 mL of liquid sample into a microwave digestion tank, adding 5mL of nitric acid, digesting the sample according to the operation steps of microwave digestion, cooling, taking out the digestion tank, dispelling acid to about 1mL on an electric hot plate at 140-160 ℃, cooling the digestion tank, transferring digestive juice into a 10mL volumetric flask, washing the digestion tank with a small amount of water for 2-3 times, combining washing liquids in the volumetric flask, fixing the volume to the scale with water, uniformly mixing for later use, and simultaneously performing a reagent blank test;
the pressure tank is used for digesting and weighing 0.2g-1g of solid sample or accurately transferring 0.500mL-5.00mL of liquid sample into a digestion inner tank, adding 5mL of nitric acid, covering an inner cover, screwing a stainless steel outer sleeve, putting the stainless steel outer sleeve into a constant temperature drying box, keeping the temperature at 140 ℃ -160 ℃ for 4h-5h, slowly unscrewing an outer tank after cooling, taking out the digestion inner tank, putting the digestion inner tank on an adjustable electric heating plate, dispelling the acid to about 1mL at 140 ℃ -160 ℃, transferring digestive juice into a 10mL volumetric flask after cooling, washing the inner tank and the inner cover for 2-3 times with a small amount of water, combining washing liquid into the volumetric flask, fixing the volume to a scale with water, mixing uniformly for later use, and simultaneously performing a reagent blank test.
In the step (5), 10 μ L of lead standard series solution and 5 μ L of ammonium dihydrogen phosphate-palladium nitrate solution are respectively injected into a graphite furnace from low mass concentration to high mass concentration, the absorbance value is measured after atomization, a standard curve is prepared by taking the mass concentration as abscissa and the absorbance value as ordinate, the sample solution is measured, 10 μ L of blank solution or sample solution and 5 μ L of ammonium dihydrogen phosphate-palladium nitrate solution are injected into the graphite furnace under the same experimental condition with the standard solution, and the absorbance value is measured after atomization and is compared with the standard series for quantification.
In the foregoing method for determining the content of lead in food, the content of lead in the sample is calculated according to the following formula:
in the formula:
x-the amount of lead in the sample in milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
rho-mass concentration of lead in the sample solution in micrograms per liter (. mu.g/L);
ρ0-mass concentration of lead in the blank solution in micrograms per liter (μ g/L);
v is the constant volume of the digestion solution of the sample, and the unit is milliliter (mL);
m-sample weighing or sample removal volume in grams or milliliters (g or mL);
1000-conversion factor.
The invention has the beneficial effects that: when the device works, a sample is digested, atomized by a graphite furnace, and the absorbance is measured at 283.3 nm. The absorbance value of the lead in a certain concentration range is in direct proportion to the lead content, and the absorbance value is compared and quantified with a standard series, so that the lead content in the food can be well measured.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1: a method for measuring the lead content in food is characterized in that: comprises the following steps of (a) carrying out,
(1) preparing a reagent and preparing the reagent;
(2) preparing a standard solution and preparing instruments and equipment;
(3) preparing a sample;
(4) carrying out pretreatment on the sample by adopting wet digestion, microwave digestion and pressure tank digestion respectively;
(5) a standard curve is prepared, and the sample solution is measured.
Preferably, in step (1), the reagent to be prepared is nitric acid (HNO)3) Perchloric acid (HClO)4) Ammonium dihydrogen phosphate (NH4H2PO4) and palladium nitrate [ Pd (NO3)2 ]]Then, the reagent is prepared,
(A1) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 950mL of water, and uniformly mixing;
(A2) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 450mL of water, and uniformly mixing;
(A3) and (3) weighing 0.02g of palladium nitrate, adding a small amount of nitric acid solution to dissolve the palladium nitrate, then adding 2g of ammonium dihydrogen phosphate, dissolving, metering the volume to 100mL by using nitric acid solution, and uniformly mixing.
Preferably, in step (2), the preparation of the standard solution comprises,
(B1) lead standard stock solution: accurately weighing 1.5985-1.6013g of lead nitrate, dissolving the lead nitrate by using a small amount of nitric acid solution, transferring the lead nitrate into a 1000mL volumetric flask, adding water to the scale, and uniformly mixing;
(B2) lead standard intermediate solution: accurately sucking 1.00mL of lead standard stock solution into a 1000mL volumetric flask, adding a nitric acid solution to a scale, and uniformly mixing;
(B3) and (3) respectively sucking 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL and 4.00mL of the lead standard intermediate solution into a 100mL volumetric flask, adding a nitric acid solution to the scales, and uniformly mixing, wherein the mass concentrations of the lead standard intermediate solution are respectively 0 mug/L, 5.00 mug/L, 10.0 mug/L, 20.0 mug/L, 30.0 mug/L and 40.0 mug/L.
Preferably, in the step (2), the apparatus and equipment comprise an atomic absorption spectrometer, an analytical balance, an adjustable electric heating furnace, an adjustable electric heating plate, a microwave digestion system, a constant temperature drying box and a pressure digestion tank.
Preferably, in step (3), samples of vegetables, fruits, fish and meat are washed with water, air-dried, and the edible part is taken, homogenized and stored in a plastic bottle.
Preferably, in the step (4), the wet digestion is as follows: weighing 0.2-3 g of solid sample or accurately transferring 0.500-5.00 mL of liquid sample into a graduated digestion tube, adding 10mL of nitric acid and 0.5mL of perchloric acid, digesting on an adjustable electric heating furnace, adding a small amount of nitric acid if the digestion solution is tan, digesting until white smoke appears, taking out the digestion tube, cooling, adding water to a constant volume of 10mL, uniformly mixing for later use, and simultaneously performing a reagent blank test;
the microwave digestion: weighing 0.2-0.8 g of solid sample or accurately transferring 0.500-3.00 mL of liquid sample into a microwave digestion tank, adding 5mL of nitric acid, digesting the sample according to the operation steps of microwave digestion, cooling, taking out the digestion tank, dispelling acid to about 1mL on an electric hot plate at 140-160 ℃, cooling the digestion tank, transferring digestive juice into a 10mL volumetric flask, washing the digestion tank with a small amount of water for 2-3 times, combining washing liquids in the volumetric flask, fixing the volume to the scale with water, uniformly mixing for later use, and simultaneously performing a reagent blank test;
microwave digestion heating meter
| Step (ii) of | Setting temperature of | Time of temperature rise min | Constant temperature time min |
| 1 | 120 | 5 | 5 |
| 2 | 160 | 5 | 10 |
| 3 | 180 | 5 | 10 |
The pressure tank is used for digesting and weighing 0.2g-1g of solid sample or accurately transferring 0.500mL-5.00mL of liquid sample into a digestion inner tank, adding 5mL of nitric acid, covering an inner cover, screwing a stainless steel outer sleeve, putting the stainless steel outer sleeve into a constant temperature drying box, keeping the temperature at 140 ℃ -160 ℃ for 4h-5h, slowly unscrewing an outer tank after cooling, taking out the digestion inner tank, putting the digestion inner tank on an adjustable electric heating plate, dispelling the acid to about 1mL at 140 ℃ -160 ℃, transferring digestive juice into a 10mL volumetric flask after cooling, washing the inner tank and the inner cover for 2-3 times with a small amount of water, combining washing liquid into the volumetric flask, fixing the volume to a scale with water, mixing uniformly for later use, and simultaneously performing a reagent blank test.
Preferably, in the step (5), 10 μ L of the lead standard solution and 5 μ L of the ammonium dihydrogen phosphate-palladium nitrate solution are respectively injected into the graphite furnace in sequence from low to high in mass concentration, the absorbance value is measured after atomization, a standard curve is prepared by taking the mass concentration as the abscissa and the absorbance value as the ordinate, the sample solution is measured, 10 μ L of the blank solution or the sample solution and 5 μ L of the ammonium dihydrogen phosphate-palladium nitrate solution are simultaneously injected into the graphite furnace under the same experimental conditions as the standard solution, and the absorbance value is measured after atomization and is compared with the standard solution for quantification.
Preferably, the lead content in the sample is calculated according to the formula:
in the formula:
x-the amount of lead in the sample in milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
rho-mass concentration of lead in the sample solution in micrograms per liter (. mu.g/L);
ρ0-mass concentration of lead in the blank solution in micrograms per liter (μ g/L);
v is the constant volume of the digestion solution of the sample, and the unit is milliliter (mL);
m-sample weighing or sample removal volume in grams or milliliters (g or mL);
1000-conversion factor.
In conclusion, in the use of the present invention, after the sample digestion treatment, the sample was atomized in a graphite furnace, and the absorbance was measured at 283.3 nm. The method comprises the steps of directly proportional measuring the lead absorbance value and the lead content in a certain concentration range, comparing and quantifying with a standard series, respectively injecting 10 mu L of lead standard series solution and 5 mu L of ammonium dihydrogen phosphate-palladium nitrate solution into a graphite furnace according to the sequence from low to high of mass concentration, measuring the absorbance value after atomization, making a standard curve by taking the mass concentration as a horizontal coordinate and the absorbance value as a vertical coordinate, measuring a sample solution, measuring the absorbance value after atomization, comparing and quantifying with the standard series, and accurately calculating the lead content in the food by using a formula.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A method for measuring the lead content in food is characterized in that: comprises the following steps of (a) carrying out,
(1) preparing a reagent and preparing the reagent;
(2) preparing a standard solution and preparing instruments and equipment;
(3) preparing a sample;
(4) carrying out pretreatment on the sample by adopting wet digestion, microwave digestion and pressure tank digestion respectively;
(5) a standard curve is prepared, and the sample solution is measured.
2. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (1), the prepared reagent is nitric acid (HNO)3) Perchloric acid (HClO)4) Ammonium dihydrogen phosphate (NH4H2PO4) and palladium nitrate [ Pd (NO3)2 ]]Then, the reagent is prepared,
(A1) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 950mL of water, and uniformly mixing;
(A2) nitric acid solution: measuring 50mL of nitric acid, slowly adding the nitric acid into 450mL of water, and uniformly mixing;
(A3) and (3) weighing 0.02g of palladium nitrate, adding a small amount of nitric acid solution to dissolve the palladium nitrate, then adding 2g of ammonium dihydrogen phosphate, dissolving, metering the volume to 100mL by using nitric acid solution, and uniformly mixing.
3. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (2), the preparation of the standard solution comprises,
(B1) lead standard stock solution: accurately weighing 1.5985-1.6013g of lead nitrate, dissolving the lead nitrate by using a small amount of nitric acid solution, transferring the lead nitrate into a 1000mL volumetric flask, adding water to the scale, and uniformly mixing;
(B2) lead standard intermediate solution: accurately sucking 1.00mL of lead standard stock solution into a 1000mL volumetric flask, adding a nitric acid solution to a scale, and uniformly mixing;
(B3) and (3) respectively sucking 0mL, 0.500mL, 1.00mL, 2.00mL, 3.00mL and 4.00mL of the lead standard intermediate solution into a 100mL volumetric flask, adding a nitric acid solution to the scales, and uniformly mixing, wherein the mass concentrations of the lead standard intermediate solution are respectively 0 mug/L, 5.00 mug/L, 10.0 mug/L, 20.0 mug/L, 30.0 mug/L and 40.0 mug/L.
4. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (2), the instruments and equipment comprise an atomic absorption spectrometer, an analytical balance, an adjustable electric heating furnace, an adjustable electric heating plate, a microwave digestion system, a constant-temperature drying box and a pressure digestion tank.
5. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (3), samples of vegetables, fruits, fishes and meats are washed by water, dried, and edible parts are taken to be prepared into homogenate and stored in a plastic bottle.
6. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (4), the wet digestion is as follows: weighing 0.2-3 g of solid sample or accurately transferring 0.500-5.00 mL of liquid sample into a graduated digestion tube, adding 10mL of nitric acid and 0.5mL of perchloric acid, digesting on an adjustable electric heating furnace, adding a small amount of nitric acid if the digestion solution is tan, digesting until white smoke appears, taking out the digestion tube, cooling, adding water to a constant volume of 10mL, uniformly mixing for later use, and simultaneously performing a reagent blank test;
the microwave digestion: weighing 0.2-0.8 g of solid sample or accurately transferring 0.500-3.00 mL of liquid sample into a microwave digestion tank, adding 5mL of nitric acid, digesting the sample according to the operation steps of microwave digestion, cooling, taking out the digestion tank, dispelling acid to about 1mL on an electric hot plate at 140-160 ℃, cooling the digestion tank, transferring digestive juice into a 10mL volumetric flask, washing the digestion tank with a small amount of water for 2-3 times, combining washing liquids in the volumetric flask, fixing the volume to the scale with water, uniformly mixing for later use, and simultaneously performing a reagent blank test;
the pressure tank is used for digesting and weighing 0.2g-1g of solid sample or accurately transferring 0.500mL-5.00mL of liquid sample into a digestion inner tank, adding 5mL of nitric acid, covering an inner cover, screwing a stainless steel outer sleeve, putting the stainless steel outer sleeve into a constant temperature drying box, keeping the temperature at 140 ℃ -160 ℃ for 4h-5h, slowly unscrewing an outer tank after cooling, taking out the digestion inner tank, putting the digestion inner tank on an adjustable electric heating plate, dispelling the acid to about 1mL at 140 ℃ -160 ℃, transferring digestive juice into a 10mL volumetric flask after cooling, washing the inner tank and the inner cover for 2-3 times with a small amount of water, combining washing liquid into the volumetric flask, fixing the volume to a scale with water, mixing uniformly for later use, and simultaneously performing a reagent blank test.
7. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: in the step (5), 10 mu L of lead standard series solution and 5 mu L of ammonium dihydrogen phosphate-palladium nitrate solution are respectively injected into a graphite furnace from low mass concentration to high mass concentration, the absorbance value is measured after atomization, a standard curve is prepared by taking the mass concentration as abscissa and the absorbance value as ordinate, the sample solution is measured, 10 mu L of blank solution or sample solution and 5 mu L of ammonium dihydrogen phosphate-palladium nitrate solution are injected into the graphite furnace under the same experimental condition with the standard solution, the absorbance value is measured after atomization, and the measurement is compared with the standard series for quantification.
8. The method for determining the lead content in the food according to claim 1, wherein the method comprises the following steps: the content of lead in the sample is calculated according to the formula:
in the formula:
x-the amount of lead in the sample in milligrams per kilogram or milligrams per liter (mg/kg or mg/L);
rho-mass concentration of lead in the sample solution in micrograms per liter (. mu.g/L);
ρ0-mass concentration of lead in the blank solution in micrograms per liter (μ g/L);
v is the constant volume of the digestion solution of the sample, and the unit is milliliter (mL);
m-sample weighing or sample removal volume in grams or milliliters (g or mL);
1000-conversion factor.
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