CN110987592A - Method for automatically and rapidly digesting food sample - Google Patents
Method for automatically and rapidly digesting food sample Download PDFInfo
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- G—PHYSICS
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Abstract
The invention discloses a method for automatically and rapidly digesting a food sample, and belongs to the technical field of food hygiene physicochemical inspection. The food sample is digested by a full-automatic graphite digestion instrument, a matched cover is required to be covered on a digestion tube in the digestion process, and the bottom 1/4-1/2 of the digestion tube body is positioned in a graphite hole for heating. The method overcomes the defects of the existing food sample digestion method, such as long digestion time by a dry method, easy pollution, inapplicability of measuring volatile elements such as arsenic, mercury, tin, selenium and the like; the method has the defects of large acid consumption, multiple acid types, long digestion time, large blank value, easy environmental pollution, inapplicability for measuring mercury element and the like in wet digestion; the microwave digestion has the defects of low risk of high-pressure tube explosion, small digestion sample amount, high labor intensity of tank screwing and cleaning, and the like.
Description
Technical Field
The invention relates to a method for automatically and rapidly digesting a food sample, belonging to the technical field of food hygiene physicochemical inspection.
Background
The analysis and determination of elements in food, and the pretreatment of samples is an important link. The present method for pretreating elements in samples determined by GB5009 series of food sanitation inspection methods (physicochemical part) is mainly digestion treatment, and aims to destroy organic matters, dissolve particulate matters, oxidize elements to be detected with various valence states into single high valence states or convert the elements into inorganic compounds which are easy to decompose, so as to obtain clear and transparent precipitate-free concentrated solution for detection and analysis, wherein the digestion treatment methods mainly comprise dry digestion, wet digestion, microwave digestion and the like, and the methods respectively have advantages and disadvantages: the dry digestion has the advantages of no or little use of chemical reagents and simple operation, and has the defects of long digestion time, easy pollution and unsuitability for measuring volatile elements such as arsenic, mercury, tin, selenium and the like; the wet digestion has the advantages of simple equipment and flexible operation, and has the defects of large acid consumption, multiple acid types, long digestion time, large blank value, easy environmental pollution, inapplicability of measuring mercury element and the like; the microwave digestion is the most widely applied digestion method at present, has the advantages of rapidness, complete decomposition, no element volatilization loss, less acid consumption and the like, but also has the defects of high-pressure tube explosion, small digestion sample amount, large labor intensity of tank screwing and cleaning and the like. The full-automatic graphite digestion method is a sample pretreatment method developed in recent years, is widely applied in the environment monitoring industry, is an improved method of wet digestion, is uniform in heating and controllable in heating temperature, can realize automation of acid addition, digestion and constant volume, greatly reduces the labor intensity of an analyst for manually preparing the digestion solution, but has the defects of large acid consumption, multiple acid use types, long digestion time, large blank value, easiness in environmental pollution, inapplicability in mercury element determination and the like in the traditional wet digestion method.
The incomplete digestion method is one of wet digestion, which removes most organic matters in a sample by using strong acid under the condition of low-temperature heating, only requires the digestion solution to be uniform, has the advantages of less acid types, less acid consumption, short digestion time and the like because the sample does not need to be completely digested, and has more reports in documents that the incomplete digestion method is adopted to determine elements such as lead, chromium, cadmium, arsenic and the like in food to obtain satisfactory results; method 3050B (acid digestion of sediment, sludge and soil) in the U.S. EPA standard is also not a complete digestion technique. However, at present, incomplete digestion methods mostly adopt open digestion and are not suitable for measuring mercury elements, a small amount of documents adopt a backflow cover to measure volatile mercury elements, such as a full-automatic graphite digestion-atomic fluorescence method for measuring arsenic and mercury in soil (an environmental monitoring central station in Maanshan city, a flare starter and the like), but the method has certain limitations in the aspects of a capping mode (in-tube pressure and backflow effect), digestion temperature, digestion time, measurement of multiple elements (particularly chromium elements) and the like.
Disclosure of Invention
In order to solve the problems, the invention utilizes a full-automatic graphite digestion instrument, adopts a digestion tube to cover for reflux, and adopts the digestion tube with 1/4-1/2 at the bottom of the tube body to be positioned in a graphite hole for heating digestion, develops a brand-new automatic rapid digestion method, realizes the digestion automation, has short digestion time, less reagent types and dosage, small environmental pollution, is suitable for measuring various elements (including volatile mercury elements) in food, and overcomes the defects of the prior food sample digestion method, such as long digestion time by a dry method, easy pollution, inapplicability for measuring the volatile elements such as arsenic, mercury, tin, selenium and the like; the wet digestion (full-automatic graphite digestion method) has the defects of large acid consumption, various acid types, long digestion time, large blank value, easy environmental pollution, inapplicability of mercury element determination and the like; the microwave digestion has the defects of low risk of high-pressure tube explosion, small digestion sample amount, high labor intensity of tank screwing and cleaning, and the like. The invention has wide measurement range and is suitable for measuring various elements such as potassium, calcium, sodium, magnesium, ferrum, manganese, zinc, copper, arsenic, lead, mercury, chromium, cadmium, selenium, nickel, phosphorus, molybdenum, vanadium and the like in food.
The invention provides a method for automatically and quickly digesting a food sample, which is to digest the food sample by using a full-automatic graphite digestion instrument, wherein a matched cover is required to be covered on a digestion tube in the digestion process, and the bottom 1/4-1/2 of the digestion tube body is positioned in a graphite hole for heating.
In one embodiment of the invention, the method comprises the steps of:
(1) weighing a sample, namely placing a polytetrafluoroethylene digestion tube with the weighed sample in a full-automatic graphite digestion instrument;
(2) adding a digestion reagent into the digestion tube with the weighed sample, covering a cover of the digestion tube, and heating for digestion;
(3) cooling after digestion, opening a digestion tube cover, fixing the volume and standing.
In one embodiment of the present invention, the cap is not completely screwed in the capping, and the cap is screwed and then turned 1/4 times, so that the purpose is:
a) keeping the positive pressure in the tube to accelerate the digestion of the sample;
b) the pressure is conveniently released under high pressure, so that the pipe is prevented from being exploded;
c) the bottom of the digestion tube is heated, the upper part is cooled at normal temperature, and the nitric acid is enabled to flow back in the tube by covering, namely, sulfuric acid with high boiling point, perchloric acid and the like are not needed to be added, the using amount of the nitric acid can be reduced, and meanwhile, the loss of volatile elements such as mercury, arsenic, selenium and the like is avoided.
In one embodiment of the invention, when the digestion tube is placed in a full-automatic graphite digestion instrument, the bottom 1/4-1/2 of the digestion tube body is positioned in a graphite hole for heating, and the purpose is as follows:
a) the bottom of the digestion tube is heated, the upper part of the digestion tube is cooled at normal temperature to generate temperature difference, and meanwhile, the nitric acid is covered to form reflux in the tube, so that the problem that the digestion of a sample is influenced due to evaporation of the nitric acid during high-temperature heating is avoided;
b) the temperature of the pipe orifice is reduced, the escape amount of acid vapor during high-temperature heating is reduced, and the loss of mercury elements is avoided.
In one embodiment of the invention, the digestion reagent is nitric acid, and the usage amount is 2.0-6.0 mL.
In one embodiment of the invention, the sample is a solid sample, a liquid sample.
In one embodiment of the present invention, the mass-to-volume ratio (g: mL) of the solid sample to nitric acid is (0.5 to 5): (2-6).
In one embodiment of the invention, the volume ratio of the liquid sample to the nitric acid is (1-5): (2-6).
In one embodiment of the present invention, the ethanol-containing liquid sample is first heated at low temperature on an electric hot plate to remove ethanol;
in one embodiment of the invention, the digestion is carried out for 20-40min at 160-200 ℃ after capping.
In one embodiment of the invention, the digestion solution is uniformly clear after digestion is complete.
In one embodiment of the invention, the method comprises the steps of:
(1) weighing a solid sample 0.5-2 g (the accuracy is 0.001g, the sample amount can be increased to 5g for samples with more water) in a polytetrafluoroethylene digestion tube, and heating the sample containing ethanol on an electric hot plate at a low temperature to remove the ethanol;
(2) placing the weighed digestion tubes in a full-automatic graphite digestion instrument, wherein the bottoms 1/4-1/2 of digestion tube bodies are positioned in graphite holes, and running a digestion program;
(3) after the instrument automatically adds the nitric acid, the cover of the digestion tube is covered, and the sample is heated and digested;
(4) and cooling after digestion, opening a tube cover of the digestion tube, running a constant volume program, keeping constant volume to 25 or 50mL, and standing.
In one embodiment of the invention, the method comprises the steps of:
(1) weighing a sample, transferring 1.00-5.00 mL of a liquid sample into a polytetrafluoroethylene digestion tube, and heating the sample containing ethanol on an electric heating plate at a low temperature to remove the ethanol;
(2) placing the weighed digestion tubes in a full-automatic graphite digestion instrument, wherein the bottoms 1/4-1/2 of digestion tube bodies are positioned in graphite holes, and running a digestion program;
(3) after the instrument automatically adds the nitric acid, the cover of the digestion tube is covered, and the sample is heated and digested;
(4) and cooling after digestion, opening the cover of the digestion tube, running a constant volume program, keeping constant volume to 25 or 50mL, and standing.
The second purpose of the invention is to provide the application of the method in food detection.
In one embodiment of the invention, the application is to detect the content of elements in food, and the application is to detect the content of elements in food by using the digestion method in combination with an atomic absorption instrument, an atomic fluorescence photometer, an inductively coupled plasma emission spectrometer and an inductively coupled plasma mass spectrometer.
In one embodiment of the invention, the elements include trace elements, macroelements and rare earth elements; the elements include potassium, calcium, sodium, magnesium, iron, manganese, zinc, copper, arsenic, lead, mercury, chromium, cadmium, selenium, nickel, phosphorus, molybdenum and vanadium.
The third purpose of the invention is to provide a method for detecting the content of food elements, which is to digest a food sample by adopting the digestion method and then detect the elements in the food sample by adopting an inductively coupled plasma mass spectrometer.
In an embodiment of the present invention, the operating parameters of the inductively coupled plasma mass spectrometer are: the radio frequency power is 1000-1500W, the atomization gas flow is 0.5-2mL/min, the auxiliary gas flow is 0.5-1mL/min, the plasma gas flow is 10-20mL/min, the analysis mode is a collision reaction pool, and the collision gas (He) flow is 3-5 mL/min.
The invention has the beneficial effects that:
1. when the cover of the digestion tube is covered, the cover is not completely screwed, and the cover can be turned for 1/4 circles after being screwed, so that the purposes are as follows: a) keeping the positive pressure in the tube to accelerate the digestion of the sample; b) the pressure is conveniently released under high pressure, so that the pipe is prevented from being exploded; c) the bottom of the digestion tube is heated, the upper part is cooled at normal temperature, and the nitric acid is enabled to flow back in the tube by covering, namely, sulfuric acid with high boiling point, perchloric acid and the like are not needed to be added, the using amount of the nitric acid can be reduced, and meanwhile, the loss of volatile elements such as mercury, arsenic, selenium and the like is avoided.
2. When the digestion pipe is arranged in a full-automatic graphite digestion instrument, the bottom 1/4-1/2 of the digestion pipe body is positioned in a graphite hole for heating, and the purpose is as follows: a) the bottom of the digestion tube is heated, the upper part of the digestion tube is cooled at normal temperature to generate temperature difference, and meanwhile, the nitric acid is covered to form reflux in the tube, so that the problem that the digestion of a sample is influenced due to evaporation of the nitric acid during high-temperature heating is avoided; b) the temperature of the pipe orifice is reduced, the escape amount of acid vapor during high-temperature heating is reduced, and the loss of mercury elements is avoided.
3. The automatic acidification, automatic digestion, automatic constant volume, time and labor saving and work efficiency improvement.
4. The digestion time is short, the types and the using amount of reagents are less, the environmental pollution is reduced, and the economic benefit and the ecological benefit are improved.
5. The digestion is convenient, and the sample weighing range is wide.
6. The digestion method is suitable for determining various elements in food, including volatile mercury elements.
7. The method overcomes the defects of the existing food sample digestion method, such as long digestion time by a dry method, easy pollution, inapplicability of measuring volatile elements such as arsenic, mercury, tin, selenium and the like; the method has the defects of large acid consumption, multiple acid types, long digestion time, large blank value, easy environmental pollution, inapplicability for measuring mercury element and the like in wet digestion; the microwave digestion has the defects of low risk of high-pressure tube explosion, small digestion sample amount, high labor intensity of tank screwing and cleaning, and the like.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
Instruments and reagents: DEENA II fully automatic graphite digestion instrument (Thomas Cain, USA), NexIon 350D inductively coupled plasma mass spectrometer (PE, USA), ME204E electronic balance (METTLER TOLEDO, Switzerland); high purity nitric acid (suzhou crystal rui chemical ltd); ICP standard solution (Ba, Be, Cd, Mg, Co, C, Cu, Mo, Pb, Tl, Zn10Mg/L, Fluka corporation), standard solution of arsenic and mercury (1Mg/mL, national center for research on Standard substances), and the use solution is diluted with 1% nitric acid step by step before use.
Example 1:
a method for automatically and rapidly digesting a food sample comprises the following specific steps:
weighing 0.5-2 g of solid sample (the accuracy is 0.001g, the sample with more water can be increased to 5g) or transferring 1.00-5.00 mL of liquid sample into a polytetrafluoroethylene digestion tube, and heating the sample containing ethanol on an electric heating plate at low temperature to remove the ethanol;
1. placing the weighed polytetrafluoroethylene digestion tube in a full-automatic graphite digestion instrument, and operating a digestion program; when the digestion pipe is placed in a full-automatic graphite digestion instrument, the bottom 1/4-1/2 of the digestion pipe body is positioned in the graphite hole for heating; 2.0-6.0 mL of high-purity nitric acid is added;
2. after the instrument automatically adds the nitric acid, the cover of the digestion tube is covered, the sample is heated and digested, and the digestion program is shown in table 1;
3. cooling after digestion, opening a digestion tube cover, operating a constant volume program, carrying out constant volume to 25 or 50mL, standing, and taking clear liquid for measurement by an atomic absorption instrument, an atomic fluorescence photometer, an inductively coupled plasma emission spectrometer, an inductively coupled plasma mass spectrometer and other instruments; and (3) taking clear liquid for measurement by an inductively coupled plasma mass spectrometer, wherein the working conditions of the instrument are shown in table 2.
Table 1 graphite digestion procedure
TABLE 2 inductively coupled plasma Mass spectrometer operating parameters
Example 2: accuracy test for analyzing GBW10049(GSB-27) welsh onion component analysis standard substance
Analytical GBW10049(GSB-27) welsh onion ingredient analytical standard was analyzed using the method of example 1, wherein the sample was digested: precisely weighing 1g (accurate to 0.001g) of GBW10049(GSB-27) green Chinese onion powder, placing the powder into a 50mL polytetrafluoroethylene digestion tube, adding 5.0mL of high-purity nitric acid, digesting according to the digestion method, and fixing the volume to 50mL by using pure water after the digestion is finished. The clear solution was taken for measurement by an inductively coupled plasma mass spectrometer, and the measurement results are shown in table 3.
Table 3 GBW10049(GSB-27) measurement results of part of elements in welsh onion (n ═ 3)
Example 3: effect of different parameter conditions on method accuracy
GBW10049(GSB-27) welsh onion ingredient assay standard was analyzed by the method of example 1 except that digestion program parameter conditions were changed. The specific parameter conditions are set in Table 4, and the measurement results are shown in Table 5.
Table 4 graphite digestion procedure
By changing the digestion parameter conditions, the method comprises the following steps: in the process of heating and digesting the sample by using concentrated nitric acid, under the condition that the obtained digestion solution is uniform and clear, most components in the sample are decomposed or transferred into an acid solution, but a small part of elements such as chromium can be transferred under a certain digestion condition (the temperature is higher than 160 ℃, the time is longer than 20min, and the using amount of the nitric acid is larger than 4 mL). The inventor finds that the digestion temperature is too low, the digestion time is too short, the digestion reagent dosage is too small, the digestion of the sample is influenced, and the measured values of partial elements are low through multiple experiments; the service life of the digestion pipe is influenced by overhigh digestion temperature; the working efficiency is affected if the digestion time is too long; the excessive consumption of the digestion reagent can increase the labor cost and the environmental pollution.
Table 5 GBW10049(GSB-27) measurement results of part of elements in welsh onion (n ═ 3)
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Example 4: method repeatability test
The method of example 1 is adopted to determine the lead-containing positive sample of the edible vegetable oil difficult to digest, the measurement is repeated for 6 times, and the determination results are shown in Table 6.
TABLE 6 lead content in a vegetable oil sample
Comparative example 1: accuracy test for analyzing GBW10049(GSB-27) welsh onion component analysis standard substance by adopting conventional full-automatic graphite digestion method
Compared with example 1, the difference is only that: the graphite digestion program (reference document: Zhenghongyan and the like, full-automatic graphite digestion-inductively coupled plasma mass spectrometry for measuring 4 heavy metal elements of copper, cadmium, zinc and chromium in biological samples of fish, shrimp and the like, and 2017, stage 1, 270-containing 274) specifically comprises the following steps: sample digestion: precisely weighing 1g (accurate to 0.001g) of GBW10049(GSB-27) green Chinese onion powder, placing the powder into a 50mL polytetrafluoroethylene digestion tube, digesting according to the digestion program in the table 7, using pure water to fix the volume to 50mL after the sample is completely digested, wherein the detection method is the same as that of the example 1, and the detection result is shown in the table 8.
TABLE 7 graphite digestion procedure
Table 8 GBW10049(GSB-27) measurement results of part of elements in welsh onion (n ═ 3)
By comparing the conventional digestion method with the digestion method of example 1, it can be seen that: the traditional full-automatic graphite digestion method obviously increases the acid use amount, the acid use type and the digestion time, and mercury element cannot be detected.
Comparative example 2:
the capping step in example 1, i.e. digestion by opening to the open, was omitted, and other conditions or parameters were the same as those in example 1, and GBW10049(GSB-27) welsh onion components were analyzed for the standard substance, as a result, nitric acid was rapidly evaporated to dryness, and the sample was not digested efficiently.
Comparative example 3:
the digestion tube in the embodiment 1 is heated with the whole tube body positioned in the graphite hole, other conditions or parameters are consistent with those of the embodiment 1, the standard substance for analyzing the components of GBW10049(GSB-27) green Chinese onion is analyzed, and as a result, the nitric acid is evaporated to dryness in about 20min, part of the sample is carbonized, and the sample is not effectively digested.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. The method for automatically and rapidly digesting the food sample is characterized in that the food sample is digested by a full-automatic graphite digestion instrument, and a cover is covered on a digestion tube in the digestion process.
2. Method according to claim 1, characterized in that it comprises the following steps:
(1) weighing a sample, namely placing a polytetrafluoroethylene digestion tube with the weighed sample in a full-automatic graphite digestion instrument;
(2) adding a digestion reagent into the digestion tube with the weighed sample, covering a cover of the digestion tube, and heating for digestion;
(3) cooling after digestion, opening a digestion tube cover, fixing the volume and standing.
3. The method of claim 1 or 2, wherein the capping is incompletely screwed.
4. The method according to claim 1 or 2, characterized in that when the digestion tube is placed in a full-automatic graphite digestion instrument for digestion, the bottom 1/4-1/2 of the digestion tube body is positioned in a graphite hole for heating.
5. The method according to any one of claims 1 to 4, wherein digestion is carried out at 160 to 200 ℃ for 20 to 40min after capping.
6. The method according to any one of claims 1 to 5, wherein the digestion reagent is nitric acid.
7. Use of the method of any one of claims 1 to 6 for food testing.
8. Use according to claim 7 for the detection of the elemental content of a food product by the method of any one of claims 1 to 6 in combination with an atomic absorption spectrometer, an atomic fluorescence spectrometer, an inductively coupled plasma emission spectrometer or an inductively coupled plasma mass spectrometer.
9. The use according to claim 8, wherein the elements include trace elements, macroelements and rare earth elements; the elements include potassium, calcium, sodium, magnesium, iron, manganese, zinc, copper, arsenic, lead, mercury, chromium, cadmium, selenium, nickel, phosphorus, molybdenum and vanadium.
10. The use according to claim 8 or 9, wherein the operating parameters of the inductively coupled plasma mass spectrometer are: the radio frequency power is 1000-1500W, the atomization gas flow is 0.5-2mL/min, the auxiliary gas flow is 0.5-1mL/min, the plasma gas flow is 10-20mL/min, the analysis mode is a collision reaction pool, and the collision gas (He) flow is 3-5 mL/min.
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| CN113030040A (en) * | 2021-02-25 | 2021-06-25 | 中国地质科学院地球物理地球化学勘查研究所 | Acid dispelling method for food sample digestion solution and detection method for selenium content in food sample |
| CN114486472A (en) * | 2022-01-27 | 2022-05-13 | 四川省农业科学院农业质量标准与检测技术研究所 | Pretreatment method for simultaneously determining multiple elements in agricultural products |
| CN115112748A (en) * | 2022-06-14 | 2022-09-27 | 永春县产品质量检验所(福建省香产品质量检验中心、国家燃香类产品质量监督检验中心(福建)) | Method for determining heavy metal content of incense products by ICP-MS (inductively coupled plasma-mass spectrometry) |
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