CN117367934A - Microwave digestion-ICP-OES (inductively coupled plasma-optical emission spectrometry) vitamin K determination 1 Method for preparing medium iron ions - Google Patents
Microwave digestion-ICP-OES (inductively coupled plasma-optical emission spectrometry) vitamin K determination 1 Method for preparing medium iron ions Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 68
- -1 iron ions Chemical class 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 58
- SHUZOJHMOBOZST-UHFFFAOYSA-N phylloquinone Natural products CC(C)CCCCC(C)CCC(C)CCCC(=CCC1=C(C)C(=O)c2ccccc2C1=O)C SHUZOJHMOBOZST-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229930003448 Vitamin K Natural products 0.000 title claims abstract description 26
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 title claims abstract description 26
- 239000011712 vitamin K Substances 0.000 title claims abstract description 26
- 235000019168 vitamin K Nutrition 0.000 title claims abstract description 26
- 150000003721 vitamin K derivatives Chemical class 0.000 title claims abstract description 26
- 229940046010 vitamin k Drugs 0.000 title claims abstract description 26
- 230000029087 digestion Effects 0.000 claims abstract description 62
- 239000002253 acid Substances 0.000 claims abstract description 27
- 239000000523 sample Substances 0.000 claims abstract description 27
- 239000012488 sample solution Substances 0.000 claims abstract description 27
- 239000011772 phylloquinone Substances 0.000 claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 19
- MBWXNTAXLNYFJB-LKUDQCMESA-N phylloquinone Chemical compound C1=CC=C2C(=O)C(C/C=C(C)/CCCC(C)CCCC(C)CCCC(C)C)=C(C)C(=O)C2=C1 MBWXNTAXLNYFJB-LKUDQCMESA-N 0.000 claims abstract description 16
- 239000012490 blank solution Substances 0.000 claims abstract description 15
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 15
- 239000012086 standard solution Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003814 drug Substances 0.000 claims abstract description 9
- 238000000120 microwave digestion Methods 0.000 claims abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 48
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 28
- 239000003085 diluting agent Substances 0.000 claims description 23
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000001514 detection method Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 7
- 229940079593 drug Drugs 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 230000002572 peristaltic effect Effects 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 9
- 230000009286 beneficial effect Effects 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 14
- 239000011550 stock solution Substances 0.000 description 8
- 150000002894 organic compounds Chemical class 0.000 description 6
- 235000019175 phylloquinone Nutrition 0.000 description 6
- MBWXNTAXLNYFJB-NKFFZRIASA-N phylloquinone Chemical compound C1=CC=C2C(=O)C(C/C=C(C)/CCC[C@H](C)CCC[C@H](C)CCCC(C)C)=C(C)C(=O)C2=C1 MBWXNTAXLNYFJB-NKFFZRIASA-N 0.000 description 6
- 229960001898 phytomenadione Drugs 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 208000032843 Hemorrhage Diseases 0.000 description 5
- ABSPRNADVQNDOU-UHFFFAOYSA-N Menaquinone 1 Natural products C1=CC=C2C(=O)C(CC=C(C)C)=C(C)C(=O)C2=C1 ABSPRNADVQNDOU-UHFFFAOYSA-N 0.000 description 5
- 238000004364 calculation method Methods 0.000 description 4
- 108010094028 Prothrombin Proteins 0.000 description 3
- 102100027378 Prothrombin Human genes 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229940039716 prothrombin Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 108010039209 Blood Coagulation Factors Proteins 0.000 description 2
- 102000015081 Blood Coagulation Factors Human genes 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003114 blood coagulation factor Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 208000009079 Bronchial Spasm Diseases 0.000 description 1
- 208000014181 Bronchial disease Diseases 0.000 description 1
- 206010006482 Bronchospasm Diseases 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000004097 bone metabolism Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229940088679 drug related substance Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229940082629 iron antianemic preparations Drugs 0.000 description 1
- 230000003859 lipid peroxidation Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000008733 trauma Effects 0.000 description 1
- 230000009278 visceral effect Effects 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a method for measuring vitamin K by microwave digestion-ICP-OES 1 A method for preparing iron ions belongs to the technical field of biological medicine, and comprises the following steps: adding nitric acid into a digestion tank for pre-digestion, starting microwave digestion, removing acid, preparing a sample solution to be tested, a method blank solution and the like; detecting the intensity response value of the iron element of each standard solution by adopting an inductively coupled plasma emission spectrometer, drawing a standard curve, obtaining the concentration of the iron element in the sample solution to be detected according to the standard curve, and then calculating the iron ion content; the invention increases the pre-digestion to lead the oily vitamin K 1 And the organic matters in the water sample are destroyed by fully digesting, so that the digested water sample is clear and transparent, pollution and instrument interference are avoided, and the digestion of a subsequent digestion program is facilitated. The pre-digestion can reduce the analysis blank value, and is favorable for accurately detecting the content of iron ions. The invention can remove acid, which is beneficial toReducing acidity and avoiding the influence of too high acidity on the service life of the instrument directly or indirectly.
Description
Technical Field
The invention relates to the technical field of biological medicine, in particular to a method for measuring vitamin K by microwave digestion-ICP-OES 1 A method for preparing the medium iron ions.
Background
Vitamin K 1 (VK 1 ) Belongs to vitamin K, also called as phytomenadione, is a fat-soluble vitamin, and is mainly characterized by phylloquinone in natureIn the form of vitamin K in green plants 1 Is rich in content, is an essential substance for synthesizing the prothrombin of the liver, and can promote carboxylation reaction of precursor substances of the prothrombin (II factor) and other coagulation factors (VIII, IX, X factor) so as to be converted into the prothrombin and the corresponding coagulation factors. The traditional Chinese medicine composition is clinically used for treating skin mucous membrane hemorrhage, visceral hemorrhage, hemorrhage after trauma operation, neonatal hemorrhage, other deep tissue hemorrhage and the like. In addition, vitamin K 1 Also participates in bone metabolism and cell growth, and has analgesic and bronchospasm relieving effects. Vitamin K 1 It can also be used as additive for multi-vitamin food.
Currently, vitamin K is considered 1 In the preparation process, the external sources such as solvent, solvent wrapping material or reaction equipment are used for introducing iron ions to lead to vitamin K 1 The crude drug often contains iron impurities, and the iron ions can be used as catalysts to catalyze vitamin K under certain conditions 1 And degradation reaction is carried out, so that impurities in the bulk drug and/or the preparation product are increased, and the quality of the bulk drug and/or the preparation product is affected. The recommended daily intake of iron element for adults is 10-15 mg, and 30mg for pregnant women. Iron itself is not toxic, but iron poisoning may also result when excessive or misadministered iron preparations are taken: the enhancement of lipid peroxidation induced by excessive iron can unbalance oxidation and antioxidant system, so vitamin K is required 1 And detecting and controlling the content of the middle iron ions. The current method for detecting metal ions is preferably an inductively coupled plasma spectrometry method for simultaneously measuring multiple elements or other methods with the sensitivity equivalent to that of the inductively coupled plasma spectrometry method.
Due to vitamin K 1 The detection sample is oily, the direct selection of the analysis method is easy to cause instrument pollution, the instrument is difficult to clean after the detection is finished, and the oily is easy to interfere with the instrument in the analysis process to cause inaccurate detection result, which is not beneficial to guaranteeing vitamin K 1 Development and effective control of production quality.
In view of the fact that there are no relevant guidelines and literature reports on the determination of iron ion content in vitamin K1, it is necessary to develop a highly accurate method to solve the above-mentioned technical difficulties.
Disclosure of Invention
The invention aims to provide a method for measuring vitamin K by microwave digestion-ICP-OES 1 The method for measuring the vitamin K in the middle iron ions is accurate, reliable, high in specificity, efficient, quick, small in reagent consumption and small in environmental pollution, and solves the problem that the vitamin K cannot be measured accurately in the prior art 1 The problem of medium iron ions.
To achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for measuring vitamin K by microwave digestion-ICP-OES 1 A method of forming Fe ions comprising the steps of:
step (1): sample pre-digestion: weighing vitamin K 1 Adding a bulk drug sample into a digestion tank, and soaking by adding nitric acid, wherein the mass-volume ratio of the sample to the strong acid is 20-30:1, a step of;
step (2): microwave digestion treatment: starting a digestion program;
step (3): acid removal and preparation of a sample solution to be tested: after digestion is finished, opening a digestion tank, and adding hydrochloric acid and hydrogen peroxide, wherein the volume ratio of the hydrogen peroxide to the strong acid in the step (1) is 1:1.2 to 5, further preferably 1:1.33-2.5; heating and acid removing the digestion tank in an acid removing device, cooling and then fixing the volume to obtain a sample solution to be measured;
step (4): the preparation method comprises the following steps: replacing a sample with deionized water, and preparing according to the methods of the steps 1 to 3 in sequence to obtain a blank solution of the method;
step (5): preparing a linear standard solution: gradually diluting with diluent to prepare iron standard solution with concentration of 0.002, 0.02, 0.1, 0.5, 1.0, 2.5 and 10 μg/L; step (6): drawing a standard curve: detecting the intensity response value of the iron element of each standard solution by adopting an inductively coupled plasma emission spectrometer, and drawing a standard curve by taking the intensity response value of the iron element as an ordinate and the concentration as an abscissa;
step (7): sample content determination: and respectively injecting the sample solution to be measured and the blank solution of the method into an inductively coupled plasma emission spectrometer (ICP-OES), measuring a signal response value of the iron element, obtaining the concentration of the iron element in the sample solution to be measured according to a standard curve, and then calculating the iron ion content.
The iron ion content calculation formula is: vitamin K 1 Middle iron ion content (ppm) =cs/Cu;
wherein C is S The concentration of iron ions in the sample solution is expressed in mug/ml; cu is the concentration of the sample solution in mg/ml.
As an embodiment of the present invention, in the step (1), the strong acid is selected from one or more of nitric acid, hydrofluoric acid, and hydrochloric acid. The strong acid is preferably nitric acid, especially preferably superior pure or electronic grade nitric acid, preferably electronic grade nitric acid.
As an embodiment of the present invention, in the step (1), the mass-to-volume ratio of the sample to the strong acid is optionally 20:1,21: 1,22: 1,23: 1,24: 1,25: 1,26: 1,27: 1,28: 1,29: 1 or 30:1.
as one embodiment of the present invention, in the step (1), the soaking time is about 10-24h, and the soaking time is selected from 11h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or 24h.
In the step (2), the digestion procedure is that, in the first step, the temperature is raised to 120 ℃ within 5min and maintained for 10min; and secondly, heating to 160 ℃ within 5min, and maintaining for 30min.
In the step (2), the digestion process is performed 2 to 4 times.
As one embodiment of the present invention, the diluent is a mixed solution of an aqueous hydrochloric acid solution and an aqueous nitric acid solution; the concentration range of the hydrochloric acid aqueous solution and the nitric acid aqueous solution is 0.5-1.5%; the concentration of the aqueous hydrochloric acid solution and the aqueous nitric acid solution can be selected to be 1%.
As one embodiment of the invention, in the step (3), the molar concentration of hydrochloric acid is in the range of 6-12mol/L, the concentration of hydrogen peroxide is in the range of 10-30%, and the acid-dispelling device is heated to the temperature range of 160-180 ℃.
As one embodiment of the invention, the molar concentration of the hydrochloric acid is 6mol/L, the concentration of the hydrogen peroxide is 15%, and the acid-driving device is heated to 170 ℃.
In one embodiment of the present invention, the acid-expelling time in the step (3) is 0.9 to 1.1 hours, preferably 1 hour.
As one embodiment of the present invention, the measurement conditions of the inductively coupled plasma emission spectrometer are,
wavelength: 259.940nm;
number of scans/repetitions: 1, a step of;
repeat times (refer to read times): 3, a step of;
detection mode: level;
peristaltic pump speed (rmp): 45;
auxiliary gas: 0.5L/min;
RF power (radio frequency power): 1150;
atomizer flow rate: 0.5L/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention develops a novel method for measuring vitamin K by microwave digestion-ICP-OES 1 In the method for removing the medium iron ions, nitric acid is selected as a digestion solution, a sample is put into a digestion tank for pre-digestion, a formal digestion procedure is carried out after the pre-digestion is completed, and hydrochloric acid and hydrogen peroxide are added for acid removal after the digestion. Nitric acid as a strong oxidant can oxidize and erode organic substances to make vitamin K 1 The medium iron ions become soluble nitrate, which is beneficial to the detection of the iron ion content by the inductively coupled plasma emission spectrometer.
2. The method adds the step of pre-digestion, can fully digest the oily vitamin K1, destroy organic matters in the oily vitamin K1 so as to release divalent/trivalent iron ions, is beneficial to clear, transparent and precipitation-free of a digested water sample, avoids pollution and interference to an instrument, and is beneficial to digestion of a subsequent digestion program. In addition, the pre-digestion can reduce the analysis blank value, is favorable for accurately detecting the content of iron ions, can eliminate instrument pollution and prolong the service life of the instrument, thereby ensuring the vitamin K 1 Development and effective control of production quality.
3. According to the method, hydrochloric acid and hydrogen peroxide are added to remove acid after the digestion procedure is finished, and the oxidation-reduction reaction between the hydrogen peroxide and the nitric acid is utilized to help remove acid better. Hydrochloric acid can react with indissolvable oxides and sulfates at high temperature to generate soluble salts, and dissolve carbonates, hydroxides, phosphates and various sulfides. In the prior art, hydrochloric acid is added in a digestion program, so that the microwave digestion instrument is corroded, and the consumption of the hydrochloric acid is required to be strictly controlled; in the invention, hydrochloric acid is added in the acid removing process without considering the limitation of a microwave digestion instrument, so that the dosage range of the hydrochloric acid has large selectivity. Acid expelling is beneficial to reducing acidity and protecting instrument and equipment, and the service life of the instrument is directly or indirectly influenced by too high acidity
The method is efficient and rapid, has strong digestion capability, saves time and labor, has little reagent consumption, saves cost and has little environmental pollution, is suitable for popularization and application, and has important significance on the safety and quality controllability of medicines.
Drawings
FIG. 1 is a standard curve of iron ions in example 1 of the present invention.
FIG. 2 is the iron ion concentration measured by ICP-OES in example 2 of the present invention.
FIG. 3 is the iron ion concentration measured by ICP-OES in example 3 of the present invention.
Detailed Description
The present invention is further described below with reference to examples, but embodiments of the present invention are not limited thereto.
Microwave digestion-ICP-OES (inductively coupled plasma-optical emission spectrometry) vitamin K determination 1 Method of neutralizing iron ions, vitamin K used in the examples 1 Drug substance samples, iron standard solutions, equipment used, or other reagents/materials are commercially available.
Example 1
The experimental conditions were as follows:
1. the device comprises: analytical balance Sartorius MSE-225S-10E-0V;
microwave digestion system Multiwace Go MULT/WAVG 053436;
inductively coupled plasma emission spectroscopy apparatus Therrno 6300NIFC.
2. Measurement conditions of inductively coupled plasma emission spectrometer (ICP-OES): wavelength: 259.940; number of scans/repetitions: 1, a step of; repeat times (refer to read times): 3, a step of; detection mode: level; peristaltic pump speed (rmp): 45; auxiliary gas: 0.5L/min; RF power (radio frequency power): 1150; atomizer flow rate: 0.5L/min.
3. Digestion procedure:
| heating time (min) | Maintenance time (min) | Temperature (. Degree. C.) |
| 5 | 10 | 120 |
| 5 | 30 | 160 |
4. Preparing a solution:
preparing a diluent: 10mL of 1% aqueous hydrochloric acid and 10mL of 1% aqueous nitric acid are removed from a 1L measuring flask, diluted with deionized water to a fixed volume to a scale, and shaken well.
Preparing a sample solution to be tested: weighing 100mg of the sample in a digestion tank, adding 5mL of electronic grade nitric acid with the purity of 70%, and soaking for 12h; starting a digestion program, and digesting 3 times by the digestion program; after digestion is finished, opening a digestion tank, adding 2mL of hydrochloric acid with the molar concentration of 12mol/L and 2mL of hydrogen peroxide with the concentration of 15%, heating the digestion tank in an acid-removing device to 170 ℃ for acid removal for 1h, transferring the digestion solution containing the sample to a clean 50mL volumetric flask after cooling, washing the digestion tank once by 5mL of diluent, merging the washing solution into the volumetric flask, and fixing the volume to scale by the diluent to obtain a sample solution to be measured;
preparing a blank solution: replacing 100mL of the sample with 0.1mL of deionized water, and preparing other sample solutions by using the same preparation method to obtain a blank solution of the method;
preparing a linear stock solution: 1mL of the iron standard solution (the concentration of iron ions is 1000 mug/mL) is precisely removed, and the iron standard solution is placed in a 50mL measuring flask, diluted with a diluent to reach a fixed volume to scale, and shaken well.
Linear standard solution-1 preparation: and precisely transferring 10 mu L of the linear stock solution into a 100mL measuring flask, diluting with a diluent to a fixed volume to a scale, and shaking uniformly. The concentration of iron ions was 0.002. Mu.g/L.
Linear standard solution-2 preparation: and precisely transferring 10 mu L of the linear stock solution into a 10mL measuring flask, diluting with a diluent to a fixed volume to a scale, and shaking uniformly. The concentration of iron ions was 0.02. Mu.g/L.
Linear standard solution-3 preparation: and precisely transferring 50 mu L of the linear stock solution into a 10mL measuring flask, diluting with a diluent to a fixed volume to a scale, and shaking uniformly. The concentration of iron ions was 0.1. Mu.g/L.
Linear standard solution-4 preparation: accurately transferring 250 mu L of the linear stock solution into a 10mL measuring flask, diluting with a diluent to a fixed volume to a scale, and shaking uniformly. The concentration of iron ions was 0.5. Mu.g/L.
Linear standard solution-5 preparation: 500 mu L of the linear stock solution is precisely removed in a 10mL measuring flask, diluted with a diluent to a fixed volume to a scale, and shaken well. The concentration of iron ions was 1.0. Mu.g/L.
Linear standard solution-6 preparation: the linear stock solution 1250 mu L is precisely removed in a 10mL measuring flask, diluted with a diluent to a fixed volume to a scale, and shaken well. The concentration of iron ions was 2.5. Mu.g/L.
Linear standard solution-7 preparation: and precisely transferring 5mL of the linear stock solution into a 10mL measuring flask, diluting with a diluent to a fixed volume to a scale, and shaking uniformly. The concentration of iron ions was 10. Mu.g/L.
5. The test method comprises the following steps:
injecting the linear standard solutions 1-7 into an inductively coupled plasma emission spectrometer, and detecting the iron element strength response value of each linear standard solution; the inductively coupled plasma emission spectrometer repeatedly reads the numerical values for 3 times, calculates the average value of the intensity response values of the iron element, and is used for drawing an iron ion standard curve, and specific data are shown in table 1:
TABLE 1 method blank solutions and response values for linear standard solutions 1-7
Drawing an iron ion standard curve by taking the intensity response value of the iron element as an ordinate and the concentration as an abscissa, and referring to figure 1 in detail; as can be seen from FIG. 1, the linear correlation coefficient is 0.999934, the deviation is small, the linear relation of the method is good, and the precision of the measurement result is high.
Respectively injecting a sample solution to be detected and a method blank solution into an inductively coupled plasma emission spectrometer, measuring a signal response value of the iron element, obtaining the concentration of the iron element in the sample solution to be detected according to an iron ion standard curve, and then calculating the iron ion content;
the iron ion content calculation formula is: iron ion content (ppm) =cs/cu×1000 in vitamin K1;
wherein CS is the concentration of iron ions in the sample solution, and the unit is mug/ml; cu is the concentration of the sample solution in mg/ml.
EXAMPLE 1 vitamin K 1 The iron ion content was calculated to be 7.8ppm.
Example 2
The preparation methods of the diluent, the sample solution to be tested and the blank solution of the method are changed, other parameters and methods are consistent with those of the embodiment 1, the specific change contents are as follows,
preparing a diluent: 10mL of 0.5% aqueous hydrochloric acid and 10mL of 0.5% aqueous nitric acid are removed from a 1L measuring flask, diluted with deionized water to a fixed volume to a scale, and shaken well.
Preparing a sample solution to be tested: weighing 100mg of the sample in a digestion tank, adding 4mL of high-grade pure nitric acid, and soaking for 24h; starting a digestion program, and digesting the digestion program for 2 times; after digestion is finished, opening a digestion tank, adding 3mL of hydrochloric acid with the molar concentration of 6mol/L and 3mL of hydrogen peroxide with the concentration of 10%, heating the digestion tank in an acid-removing device to 160 ℃ for acid removal for 0.9h, transferring the digestion solution containing the sample to a clean 50mL volumetric flask after cooling, washing the digestion tank once by 5mL of diluent, merging the washing solution into the volumetric flask, and fixing the volume to scale by the diluent to obtain a sample solution to be measured;
preparing a blank solution: replacing 100mL of the sample with 0.1mL of deionized water, and preparing other sample solutions by using the same preparation method to obtain a blank solution of the method;
EXAMPLE 2 vitamin K 1 The iron ion content was calculated to be 6.1ppm.
Example 3
The preparation methods of the diluent, the sample solution to be tested and the blank solution of the method are changed, other parameters and methods are consistent with those of the embodiment 1, the specific change contents are as follows,
preparing a diluent: 10mL of 1.5% aqueous hydrochloric acid solution and 10mL of 1.5% aqueous nitric acid solution are removed, diluted with deionized water to a fixed volume to a scale, and shaken well.
Preparing a sample solution to be tested: weighing 100mg of the sample in a digestion tank, adding 3.5mL of high-grade pure nitric acid, and soaking for 10h; starting a digestion program, and digesting for 4 times by the digestion program; after digestion is finished, opening a digestion tank, adding 2mL of hydrochloric acid with the molar concentration of 10mol/L and 2mL of hydrogen peroxide with the concentration of 30%, heating the digestion tank in an acid-removing device to 180 ℃ for acid removal for 1.1h, transferring the digestion solution containing the sample to a clean 50mL volumetric flask after cooling, washing the digestion tank once by 5mL of diluent, merging the washing solution into the volumetric flask, and fixing the volume to scale by the diluent to obtain a sample solution to be measured;
preparing a blank solution: replacing 100mL of the sample with 0.1mL of deionized water, and preparing other sample solutions by using the same preparation method to obtain a blank solution of the method;
EXAMPLE 3 vitamin K 1 The iron ion content calculation was 8.2ppm.
Comparative example 1
Compared with example 1, the other operations are the same as example 1, dimensionBiotin K 1 The iron ion content calculation was 0.38ppm. This result is far smaller than the value of example 1, and the detection result is inaccurate, compared with example 1.
Vitamin K 1 The method is characterized in that the method comprises the steps of adding sulfuric acid into the organic compound to perform pre-digestion, soaking the organic compound for a long time under the action of a strong oxidant to destroy the molecular structure of the organic compound, decomposing the organic compound into gaseous state to release iron ions to be detected, and not performing the pre-digestion, wherein the macromolecular organic compound wraps the iron ions, so that the macromolecular organic compound cannot be fully dissolved in a diluent, the detection of the iron ions is interfered, and the detection content of the iron ions is far smaller than the actual content in a sample, so that the detection result is inaccurate.
Claims (10)
1. Microwave digestion-ICP-OES (inductively coupled plasma-optical emission spectrometry) vitamin K determination 1 A method for neutralizing iron ions, comprising the steps of:
step (1): sample pre-digestion: weighing vitamin K 1 Adding a bulk drug sample into a digestion tank, and soaking by adding strong acid, wherein the mass-volume ratio of the sample to the strong acid is 20-30:1, a step of;
step (2): microwave digestion treatment: starting a digestion program;
step (3): acid removal and preparation of a sample solution to be tested: after digestion is finished, opening a digestion tank, and adding hydrochloric acid and hydrogen peroxide, wherein the volume ratio of the hydrogen peroxide to the strong acid in the step (1) is 1:1.2-5; heating and acid removing the digestion tank in an acid removing device, cooling and then fixing the volume to obtain a sample solution to be measured;
step (4): the preparation method comprises the following steps: replacing a sample with equivalent deionized water, and preparing sequentially according to the methods from the step 1 to the step 3 to obtain a blank solution of the method;
step (5): preparing a linear standard solution: gradually diluting with diluent to prepare iron standard solution with concentration of 0.002, 0.02, 0.1, 0.5, 1.0, 2.5 and 10 μg/L;
step (6): drawing a standard curve: detecting the intensity response value of the iron element of each standard solution by adopting an inductively coupled plasma emission spectrometer, and drawing a standard curve by taking the intensity response value of the iron element as an ordinate and the concentration as an abscissa;
step (7): sample content determination: and respectively injecting the sample solution to be measured and the blank solution of the method into an inductively coupled plasma emission spectrometer, measuring a signal response value of the iron element, obtaining the concentration of the iron element in the sample solution to be measured according to a standard curve, and then calculating the iron ion content.
2. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (1), the strong acid is selected from one or more of nitric acid, hydrofluoric acid and hydrochloric acid.
3. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (1), the mass-volume ratio of the sample to the strong acid is 25:1.
4. a microwave digestion-ICP-OES assay for vitamin K according to any one of claims 1-3 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (1), the soaking time is 10-24 hours.
5. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (2), the digestion procedure is that in the first step, the temperature is raised to 120 ℃ within 5min, and the temperature is kept for 10min; and secondly, heating to 160 ℃ within 5min, and maintaining for 30min.
6. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (2), the digestion program is digested for 2-4 times.
7. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: the saidIn the step (3), the molar concentration range of hydrochloric acid is 6-12mol/L, the concentration range of hydrogen peroxide is 10-30%, and the acid-driving device is heated to 160-180 ℃.
8. A microwave digestion-ICP-OES assay for vitamin K according to claim 7 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: the molar concentration of hydrochloric acid is 6mol/L, the concentration of hydrogen peroxide is 15%, and the acid-expelling device is heated to 170 ℃.
9. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: in the step (3), the acid expelling time is 0.9-1.1h, preferably 1h.
10. A microwave digestion-ICP-OES assay for vitamin K according to claim 1 1 The method for preparing the medium iron ions is characterized by comprising the following steps of: the measurement conditions of the inductively coupled plasma emission spectrometer are that,
wavelength: 259.940;
number of scans/repetitions: 1, a step of;
number of repetitions: 3, a step of;
detection mode: level;
peristaltic pump speed (rmp): 45;
auxiliary gas: 0.5L/min;
RF power (radio frequency power): 1150;
atomizer flow rate: 0.5L/min.
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