CN104977193B - In a kind of infant food and dairy products the sample-pretreating method of detection of content of element and use its detection method - Google Patents
In a kind of infant food and dairy products the sample-pretreating method of detection of content of element and use its detection method Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 43
- 235000013365 dairy product Nutrition 0.000 title claims abstract description 22
- 235000008452 baby food Nutrition 0.000 title claims abstract description 21
- 239000000470 constituent Substances 0.000 claims abstract description 14
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 44
- 238000002203 pretreatment Methods 0.000 claims description 27
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 22
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 22
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 22
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 22
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 22
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011575 calcium Substances 0.000 claims description 22
- 229910052791 calcium Inorganic materials 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 22
- 239000011777 magnesium Substances 0.000 claims description 22
- 229910052749 magnesium Inorganic materials 0.000 claims description 22
- 229910052748 manganese Inorganic materials 0.000 claims description 22
- 239000011572 manganese Substances 0.000 claims description 22
- 239000011591 potassium Substances 0.000 claims description 22
- 229910052700 potassium Inorganic materials 0.000 claims description 22
- 239000011734 sodium Substances 0.000 claims description 22
- 229910052708 sodium Inorganic materials 0.000 claims description 22
- 239000011701 zinc Substances 0.000 claims description 22
- 229910052725 zinc Inorganic materials 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000009616 inductively coupled plasma Methods 0.000 claims description 3
- 229910001410 inorganic ion Inorganic materials 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims 2
- 239000012898 sample dilution Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 description 27
- 238000004380 ashing Methods 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 18
- 235000013350 formula milk Nutrition 0.000 description 18
- 239000002245 particle Substances 0.000 description 13
- ZDDKZHCVHSMMQM-UHFFFAOYSA-N [Mn].[Fe].[Na].[K].[Mg].[Ca].[Zn] Chemical compound [Mn].[Fe].[Na].[K].[Mg].[Ca].[Zn] ZDDKZHCVHSMMQM-UHFFFAOYSA-N 0.000 description 9
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 9
- 238000012544 monitoring process Methods 0.000 description 9
- 229910052573 porcelain Inorganic materials 0.000 description 9
- 238000011282 treatment Methods 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000002956 ash Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
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- 238000001816 cooling Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 239000003738 black carbon Substances 0.000 description 2
- 210000000481 breast Anatomy 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000006193 liquid solution Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241001536352 Fraxinus americana Species 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
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- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- 238000010183 spectrum analysis Methods 0.000 description 1
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Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a kind of sample-pretreating method of detection of content of element in infant food and dairy products, it is 5% 10% salpeter solution including adding volumn concentration in the sample, heated after obtaining mixed liquor, the state of liquid formation solid-liquor separation to be mixed, then carbonized and be ashed successively.Present invention also offers the detection method of constituent content in the infant food and dairy products using above-mentioned sample-pretreating method, it is more accurate that testing result is compared with art methods, analysis time can also be shortened, the labor intensity of staff is reduced, and save mass energy.
Description
Technical field
The present invention relates to a kind of sample-pretreating method of food inspection, in more particularly to a kind of infant food and dairy products
The sample-pretreating method of detection of content of element and use its detection method.
Background technology
Atomic absorption spectrophotometry（AAS methods）It is the ground state atom based on element to be measured in steam phase to its resoance radiation
Absorption intensity determine a kind of instrument analytical method of the constituent content of this in sample, be to determine having for trace and ultratrace element
Efficacious prescriptions method.For the measure of constituent content in infant food and dairy products, sample must decompose organic matter first through dry ashing
Afterwards, acid adding makes the inorganic ions in ash content all dissolve, and can just be directly sucked in atomization in Air-acetylene Flame, and in light
Absorption of the atom to be measured to specific wavelength spectral line is determined in road respectively.
Inductively coupled plasma atomic emission spectrometry（Inductively coupled plasma atomic
Emission spectroscopy, abridge ICP-AES）, it is to utilize the light for being coupled by high-frequency inductor and producing plasma discharge
Source is come the method that carries out Atomic Emission Spectral Analysis.Instrument mainly includes plasma torch pipe, radio-frequency generator（Produce high-frequency electrical
Stream）, induction coil, air supply system and atomization system.Torch pipe is made up of three layers of concentric quartz tubes.The argon gas being tangentially passed through in outer tube is
Plasma operation gas or cooling gas.The argon gas that middle pipe is passed through is auxiliary gas.Argon gas in inner tube is carrier gas, by sample aerosol
It is introduced into torch.For the measure of constituent content in infant food and dairy products, sample also must be diluted to conjunction first through dry ashing
After fit product, it could be determined with inductively coupled plasma atomic emission spectrometer.
Dry ashing is the important pre-treatment step of above-mentioned analysis method.Existing dry ashing method is will be well mixed
Solid sample or liquor sample in crucible, low baking temperature is carbonized to no longer smoldering on electric furnace, then moves into 490 DEG C of ashes in Muffle furnace
Change about 5 hours.If black carbon granule, after cooling, then 50% is added dropwise（V/V）Salpeter solution is a little（Sample may occur for this step
Splash) moistening.After small fire is evaporated on electric furnace, then moves into stove and continue to be ashed into white ashes.
During dry ashing, the reason such as newborn surface tension and the viscosity of breast makes heated rear easily bubble or even overflowed, breast
Middle free water and do not allow volatile with reference to water, make evaporation time long, and it is fat with albumen etc. to be evaporated the sample after moisture content
Conjugate.These physicochemical properties of dairy products in itself make it that the effect of existing method dry ashing is often undesirable.In practical operation,
For the first time ashing often contain black carbon granule, it is necessary to be repeated it is secondary, or even repeatedly ashing；Not only cause time, manpower
With the waste on the energy, the possibility for the loss introduced other pollutions or cause element also add.
The content of the invention
It is an object of the invention to provide a kind of sample-pretreating method of detection of content of element in infant food and dairy products,
It will not produce black particle in carbonization process, it is to avoid sample ashing not exclusively caused by secondary ashing.
The present invention's a further object is the detection method for providing constituent content in a kind of infant food and dairy products, and it is examined
Survey result more accurate quick.
The invention discloses a kind of sample-pretreating method of detection of content of element in infant food and dairy products, it is included in
The salpeter solution that volumn concentration is 5%-10% is added in sample, mixed liquor, the shape of liquid formation solid-liquor separation to be mixed is obtained
Heated after state, then carbonized and be ashed successively.
A kind of exemplary embodiment of the sample-pretreating method of detection of content of element in infant food and dairy products
In, the salpeter solution consumption that every gram of sample needs is 0.3mL-0.5mL.
The invention also discloses a kind of detection method of constituent content in infant food and dairy products, first pass through the present invention's
Sample-pretreating method carries out pre-treatment, obtains ash content, and then acid adding makes the inorganic ions in ash content all dissolve, and with atom
Absorption spectrophotometer determines absorption of the atom to be measured to specific wavelength spectral line respectively.
In infant food and dairy products in a kind of exemplary embodiment of the detection method of constituent content, element bag
Include：Calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese.
The invention also discloses a kind of detection method of constituent content in infant food and dairy products, first pass through the present invention's
Sample-pretreating method carries out pre-treatment, then dilutes the sample obtained after pre-treatment, then former with inductively coupled plasma
Sub- emission spectrometer is determined.
In infant food and dairy products in a kind of exemplary embodiment of the detection method of constituent content, element bag
Include：Calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese.
The sample-pretreating method that the present invention is provided, after the heating fluid sample evaporate rapidly, make the solid of caking quick
Charing, and charing is complete, and black smoke is not had when Muffle furnace is ashed, black particle will not be also produced, it is to avoid sample ashing
Secondary ashing caused by not exclusively.The time carbonized on electric hot plate is so not only saved but also charing is complete, so in ash
Sample is set fully to be ashed the pollution and loss that avoids and may be introduced in secondary podzolic process during change, more can ensuring inspection
As a result accuracy；Analysis time can also be shortened（20%-73% can be shortened）, the labor intensity of staff is reduced, and save
Mass energy（67%-92% can be saved）.
The detection method of constituent content, inspection is compared with art methods in infant food and dairy products that the present invention is provided
Survey the more accurate quick of result.
Embodiment
In order to be more clearly understood to the technical characteristic of invention, purpose and effect, illustrate in conjunction with following examples
The embodiment of the present invention.
The instrument detection of following examples sample can use arbitration law（AAS methods）, it is applied equally to the inspection of ICP-AES methods
Survey.
Embodiment 1.
1st, sample pre-treatments：Children's formula is weighed respectively（Liquid）Sample 15.0050,14.9855g（Parallel sample）
In porcelain crucible, volumn concentration is added for 10% salpeter solution 4.5mL, the state of observation mixed liquor formation solid-liquor separation
After be heated to doing, then turn big fire and carbonized and be ashed successively, black particle do not occur, 20% hydrochloric acid of the sample after ashing
Solution solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 120 | 140 | 42.5 | 8.25 | 0.809 | 1.28 | 54.1 |
| 2 | 122 | 138 | 43.2 | 8.27 | 0.812 | 1.20 | 53.9 |
| 3 | 123 | 139 | 43.0 | 8.02 | 0.805 | 1.30 | 52.9 |
| 4 | 119 | 143 | 40.9 | 8.11 | 0.810 | 1.23 | 54.0 |
| 5 | 118 | 138 | 42.9 | 8.15 | 0.842 | 1.25 | 53.5 |
| 6 | 122 | 137 | 39.5 | 8.18 | 0.830 | 1.31 | 54.0 |
| 7 | 123 | 141 | 40.8 | 8.20 | 0.826 | 1.31 | 52.9 |
| Standard deviation S | 2.0 | 2.07 | 1.43 | 0.085 | 0.0137 | 0.043 | 0.52 |
| RSD% | 1.65% | 1.48% | 3.41% | 1.05% | 1.67% | 3.38% | 0.98% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 103.2% | 98.6% | 99.5% | 95.8% | 97.2% | 102.2% | 93.9% |
Embodiment 2.
1st, sample treatment：Weigh children's formula（Liquid）Sample 14.9920,15.0152g are in porcelain crucible, then add
Enter volumn concentration for 5% salpeter solution 7.5ml, be again heated to dry after the state of observation mixed liquor formation solid-liquor separation, turn big
Live charcoal.Carbonized and be ashed successively, black particle do not occur, the sample after ashing is with 20% hydrochloric acid solution solution transfer
Constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 119 | 141 | 43.5 | 8.26 | 0.781 | 1.31 | 55.0 |
| 2 | 121 | 137 | 42.9 | 8.12 | 0.753 | 1.35 | 55.6 |
| 3 | 118 | 138 | 41.8 | 8.30 | 0.761 | 1.29 | 54.2 |
| 4 | 118 | 137 | 40.9 | 8.19 | 0.776 | 1.32 | 53.9 |
| 5 | 120 | 142 | 41.6 | 8.33 | 0.771 | 1.30 | 54.0 |
| 6 | 121 | 143 | 42.5 | 8.26 | 0.762 | 1.33 | 52.9 |
| 7 | 120 | 140 | 41.6 | 8.20 | 0.769 | 1.32 | 53.1 |
| Standard deviation S | 1.27 | 2.43 | 0.89 | 0.0718 | 0.00959 | 0.0198 | 0.96 |
| RSD% | 1.06% | 1.74% | 2.12% | 0.87% | 1.25% | 1.50% | 1.78% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 100.5% | 103.0% | 98.2% | 96.8% | 95.9% | 100.8% | 103.5% |
Embodiment 3.
1st, sample treatment：Weigh children's formula（Liquid）Sample 15.0501,15.0111g are in porcelain crucible, then add
Enter volumn concentration for 7% salpeter solution 6ml, after the state of observation mixed liquor formation solid-liquor separation（Stand 3-5 minutes）Again plus
Heat turns big fire charing to dry.Carbonized and be ashed successively, black particle do not occur, the sample after ashing is molten with 20% hydrochloric acid
Liquid solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 122 | 145 | 45.2 | 7.96 | 0.625 | 1.33 | 49.8 |
| 2 | 125 | 141 | 43.6 | 8.06 | 0.631 | 1.39 | 47.9 |
| 3 | 125 | 142 | 42.9 | 7.86 | 0.629 | 1.29 | 49.1 |
| 4 | 126 | 143 | 43.1 | 8.10 | 0.630 | 1.31 | 46.8 |
| 5 | 123 | 146 | 44.6 | 8.11 | 0.640 | 1.37 | 47.6 |
| 6 | 124 | 143 | 45.0 | 8.06 | 0.637 | 1.31 | 48.2 |
| 7 | 126 | 144 | 43.9 | 7.92 | 0.641 | 1.36 | 49.2 |
| Standard deviation S | 1.51 | 1.72 | 0.91 | 0.097 | 0.0061 | 0.037 | 1.00 |
| RSD% | 1.22% | 1.20% | 2.07% | 1.21% | 0.96% | 2.76% | 2.07% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 101.5% | 99.1% | 96.5% | 95.0% | 96.6% | 95.8% | 93.81% |
Embodiment 4.
1st, sample treatment：Weigh infant formula（Solid）Sample 5.0050,5.0331g are added in porcelain crucible
Volumn concentration is 5% salpeter solution 6ml, and observation mixed liquor is formed after the state of solid-liquor separation（Stand 3-5 minutes）Reheat
To dry, turn big fire charing.Carbonized and be ashed successively, black particle do not occur, 20% hydrochloric acid solution of the sample after ashing
Solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 456 | 668 | 207 | 73.2 | 4.56 | 5.06 | 105 |
| 2 | 460 | 671 | 210 | 74.1 | 4.26 | 5.11 | 110 |
| 3 | 450 | 652 | 206 | 73.9 | 4.38 | 5.13 | 101 |
| 4 | 462 | 656 | 203 | 73.5 | 4.50 | 5.01 | 106 |
| 5 | 455 | 670 | 211 | 72.6 | 4.42 | 5.05 | 103 |
| 6 | 462 | 653 | 209 | 73.1 | 4.32 | 5.10 | 102 |
| 7 | 469 | 660 | 211 | 72.8 | 4.29 | 5.19 | 109 |
| Standard deviation S | 6.12 | 8.16 | 2.97 | 0.55 | 0.11 | 0.059 | 3.44 |
| RSD% | 1.33% | 1.23% | 1.43% | 0.75% | 2.53% | 1.16% | 3.27% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 100.5% | 102.1% | 99.8% | 97.5% | 95.8% | 96.9% | 95.1% |
Embodiment 5.
1st, sample treatment：Weigh infant formula（Solid）Sample 5.0900,5.0062g are added in porcelain crucible
Volumn concentration is 10% salpeter solution 4ml, and observation mixed liquor is formed after the state of solid-liquor separation（Stand 3-5 minutes）Again plus
Heat turns big fire charing to dry.Carbonized and be ashed successively, black particle do not occur, the sample after ashing is molten with 20% hydrochloric acid
Liquid solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 461 | 659 | 203 | 75.0 | 4.46 | 5.21 | 110 |
| 2 | 454 | 665 | 211 | 74.6 | 4.26 | 5.29 | 109 |
| 3 | 453 | 652 | 207 | 73.5 | 4.28 | 5.18 | 105 |
| 4 | 460 | 659 | 206 | 72.9 | 4.53 | 5.13 | 101 |
| 5 | 455 | 672 | 213 | 76.1 | 4.48 | 5.15 | 106 |
| 6 | 456 | 662 | 211 | 75.1 | 4.32 | 5.15 | 102 |
| 7 | 459 | 665 | 208 | 74.8 | 4.61 | 5.18 | 105 |
| Standard deviation S | 3.13 | 6.27 | 3.45 | 1.06 | 0.135 | 0.0535 | 3.31 |
| RSD% | 0.69% | 0.95% | 1.66% | 1.43% | 3.04% | 1.03% | 3.14% |
4. the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 97.2% | 95.8% | 97.2% | 98.2% | 96.8% | 95.2% | 94.9% |
Embodiment 6.
1st, sample treatment：Weigh infant formula（Solid）Sample 4.9982,5.0121g are added in porcelain crucible
Volumn concentration is 7% salpeter solution 5ml, and observation mixed liquor is formed after the state of solid-liquor separation（Stand 3-5 minutes）Reheat
To dry, turn big fire charing.Carbonized and be ashed successively, black particle do not occur, 20% hydrochloric acid solution of the sample after ashing
Solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 465 | 661 | 212 | 72.1 | 4.66 | 5.50 | 105 |
| 2 | 460 | 655 | 209 | 73.9 | 4.36 | 5.52 | 111 |
| 3 | 450 | 649 | 210 | 76.5 | 4.58 | 5.38 | 115 |
| 4 | 453 | 661 | 216 | 74.9 | 4.43 | 5.31 | 110 |
| 5 | 455 | 680 | 206 | 72.6 | 4.68 | 5.59 | 107 |
| 6 | 465 | 672 | 206 | 76.3 | 4.44 | 5.45 | 115 |
| 7 | 466 | 669 | 211 | 76.1 | 4.56 | 5.19 | 112 |
| Standard deviation S | 6.52 | 10.6 | 3.51 | 1.81 | 0.122 | 0.137 | 3.77 |
| RSD% | 1.42% | 1.59% | 1.67% | 2.42% | 2.70% | 2.53% | 3.41% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 96.6% | 97.2% | 98.1% | 102% | 104% | 102% | 106% |
Embodiment 7.
1st, sample treatment：Weigh infant formula（Solid）Sample 4.9982,5.0121g are added in porcelain crucible
Volumn concentration is 7% salpeter solution 5ml, and observation mixed liquor is formed after the state of solid-liquor separation（Stand 3-5 minutes）Reheat
To dry, turn big fire charing.Carbonized and be ashed successively, black particle do not occur, 20% hydrochloric acid solution of the sample after ashing
Solution transfer constant volume.Pretreatment process takes：80-120 minutes；Consume the energy：3-5 KW（Electric energy）.
2nd, detect：The sample after pre-treatment is detected with ICP-AES methods, testing result is with the flat of two parallel samples
Average is represented.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 468 | 670 | 210 | 72.8 | 4.60 | 5.51 | 103 |
| 2 | 452 | 653 | 219 | 72.8 | 4.38 | 5.59 | 111 |
| 3 | 459 | 646 | 198 | 71.5 | 4.62 | 5.35 | 106 |
| 4 | 445 | 651 | 210 | 73.2 | 4.39 | 5.42 | 111 |
| 5 | 439 | 680 | 209 | 73.0 | 4.65 | 5.55 | 103 |
| 6 | 459 | 666 | 195 | 74.3 | 4.49 | 5.48 | 110 |
| 7 | 473 | 656 | 213 | 73.3 | 4.52 | 5.31 | 100 |
| Standard deviation S | 2.08 | 1.52 | 3.09 | 0.83 | 0.108 | 0.103 | 4.46 |
| RSD% | 2.65% | 1.83% | 4.04% | 1.139% | 2.40% | 1.89% | 4.20% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 98.2% | 96.9% | 97.5% | 101% | 103% | 98.3% | 98.0% |
Comparative example 1.
1st, sample treatment：Weigh children's formula（Liquid）Sample 15.0050,14.9855g are in porcelain crucible, heating
To dry, turn big fire charing.Carbonized and be ashed successively, find there is black particle appearance in sample.There is the sample of black particle
Add 5ml, 50% nitric acid on product, heating evaporation is put into Muffle furnace ashing 1h to dry, determined after cooling with 20% hydrochloric acid solution solution transfer
Hold.Pretreatment process takes：150-300 minutes；Consume the energy：15-39 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 107 | 135 | 45.6 | 8.09 | 0.601 | 1.26 | 56.2 |
| 2 | 115 | 141 | 50.0 | 8.66 | 0.639 | 1.35 | 60.1 |
| 3 | 106 | 144 | 48.6 | 8.79 | 0.621 | 1.19 | 62.1 |
| 4 | 109 | 138 | 46.2 | 8.26 | 0.646 | 1.39 | 60.3 |
| 5 | 111 | 139 | 48.2 | 8.39 | 0.651 | 1.28 | 55.1 |
| 6 | 113 | 142 | 45.9 | 8.45 | 0.644 | 1.19 | 61.8 |
| 7 | 106 | 145 | 47.2 | 8.62 | 0.619 | 1.11 | 58.6 |
| Standard deviation S | 3.55 | 3.50 | 1.62 | 0.243 | 0.182 | 0.978 | 2.69 |
| RSD% | 3.24% | 2.49% | 3.43% | 2.878% | 2.89% | 7.80% | 4.54% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 107% | 93.1% | 90.2% | 108% | 108% | 109% | 105% |
Comparative example 2.
1st, sample treatment：Infant formula sample 5.0050,5.0331g are weighed in porcelain crucible, is heated to doing, turns big
Live charcoal.Carbonized and be ashed successively, find there is black particle appearance in sample.On the sample for have black particle plus 5ml,
50% nitric acid, heating evaporation is put into Muffle furnace ashing 1h to dry, with 20% hydrochloric acid solution solution transfer constant volume after cooling.Pre-treatment
Journey takes：150-300 minutes；Consume the energy：15-39 KW（Electric energy）.
2nd, detect：With AAS methods（National standard arbitration law is atomic absorption spectrophotometry）Sample after pre-treatment is examined
Survey, testing result is represented with the average value of two parallel samples.
3rd, precision is detected：Detection seven is repeated to children's formula according to the pre-treatment and detection method of the present embodiment
It is secondary, its precision is calculated according to result, represented with RSD% values, such as following table：
| Element and detection number of times | Calcium mg/100g | Potassium mg/100g | Sodium mg/100g | Magnesium mg/100g | Zinc mg/100g | Iron mg/100g | Manganese μ g/100g |
| 1 | 480 | 652 | 209 | 69.2 | 4.09 | 5.81 | 106 |
| 2 | 462 | 610 | 198 | 72.1 | 4.45 | 5.60 | 110 |
| 3 | 445 | 672 | 206 | 73.0 | 4.84 | 5.20 | 109 |
| 4 | 439 | 631 | 210 | 68.1 | 4.30 | 5.41 | 103 |
| 5 | 472 | 625 | 192 | 66.8 | 4.16 | 5.62 | 105 |
| 6 | 433 | 630 | 205 | 70.5 | 4.29 | 5.55 | 101 |
| 7 | 452 | 643 | 193 | 64.9 | 4.22 | 5.90 | 105 |
| Standard deviation S | 17.4 | 20.2 | 7.47 | 2.89 | 0.250 | 0.235 | 3.15 |
| RSD% | 3.82% | 3.16% | 3.70% | 4.17% | 5.768% | 4.21% | 3.00% |
4th, the rate of recovery：Several elements carry out rate of recovery monitoring respectively, and the spiked levels of wherein element are respectively the mg/ of calcium 100
100g, the mg/100g of potassium 120, the mg/100g of sodium 40, the mg/100g of magnesium 8.00, the mg/100g of zinc 0.5, the mg/100g of iron 1.00,
The mg/100g of manganese 0.05, as a result such as following table：
| Calcium | Potassium | Sodium | Magnesium | Zinc | Iron | Manganese | |
| Rate of recovery % | 108% | 90.5% | 88.9% | 93.4% | 95.0% | 107% | 90.3% |
Herein, " schematic " expression " serving as example, example or explanation ", will should not be described herein as " showing
Any embodiment of meaning property " is construed to a kind of preferred or more advantageous technical scheme.
Herein, the limitation on the mathematics and/or geometry meaning of " equal ", " identical " etc. and non-critical, is also included
It will be appreciated by those skilled in the art that and production or the error for the permission such as using.Unless otherwise indicated, numerical value model herein
Enclosing not only includes the gamut in two end points, also including being contained in some subranges therein.
It should be understood that, although this specification is described according to each embodiment, but not each embodiment only includes one
Individual independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art will should say
Bright book is as an entirety, and the technical solutions in the various embodiments may also be suitably combined, and forming those skilled in the art can be with
The other embodiment of understanding.
The a series of detailed description of those listed above illustrating only for the possible embodiments of the present invention,
They simultaneously are not used to limit the scope of the invention, all equivalent embodiments made without departing from skill spirit of the present invention or change
More, such as feature combination, segmentation or repetition, should be included in the scope of the protection.
Claims (5)
1. the sample-pretreating method of detection of content of element in a kind of infant food and dairy products, it is characterised in that be included in sample
The salpeter solution that volumn concentration is 5%-10% is added in product, mixed liquor is obtained, the mixed liquor formation solid-liquor separation is treated
Heated after state, then carbonized and be ashed successively；The salpeter solution consumption that the wherein every gram sample needs is
0.3mL-0.5mL。
2. the detection method of constituent content in a kind of infant food and dairy products, it is characterised in that first pass through described in claim 1
Sample-pretreating method carry out pre-treatment, obtain ash content, then acid adding makes inorganic ions in the ash content all dissolve, and
Determine absorption of the atom to be measured to specific wavelength spectral line respectively with atomic absorption spectrophotometer.
3. the detection method of constituent content in infant food according to claim 2 and dairy products, wherein described element
Including：Calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese.
4. the detection method of constituent content in a kind of infant food and dairy products, it is characterised in that first pass through described in claim 1
Sample-pretreating method carry out pre-treatment, sample dilution then will be obtained after the pre-treatment, then inductively coupled plasma is used
Body Atomic Emission Spectrometer AES is determined.
5. the detection method of constituent content in infant food according to claim 4 and dairy products, wherein described element
Including：Calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese.
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