CN115825211A - Universal detection method for 10 element impurities in bulk drugs - Google Patents
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- CN115825211A CN115825211A CN202211664670.4A CN202211664670A CN115825211A CN 115825211 A CN115825211 A CN 115825211A CN 202211664670 A CN202211664670 A CN 202211664670A CN 115825211 A CN115825211 A CN 115825211A
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Abstract
The invention relates to the technical field of medical analysis, provides a general detection method for 10 element impurities in bulk drugs, and solves the problems of low separation degree, long detection time, low accuracy and the like of the existing detection method. The method comprises the following steps: preparing a solvent; (2) preparing a mixed reference substance stock solution; (3) preparing a mixed internal standard stock solution; (4) preparing a standard curve solution of a reference substance; (5) preparing a test solution; (6) preparing a reagent blank solution; and (7) detecting. The detection method provided by the invention is a universal method aiming at the element impurities in the raw material medicines, and has the advantages of good repeatability, high accuracy and the like.
Description
Technical Field
The invention relates to the technical field of medical analysis, in particular to a general detection method for 10 element impurities in bulk drugs.
Background
The elemental impurities in the raw material drugs have various potential sources, which may occur in any link of the raw material drug process, such as in the synthesis process, the use of catalysts (such as iridium, palladium, platinum, rhodium, etc.) or combinations of metals and metalloids; as another example, during processing, drugs are introduced inadvertently by interacting with equipment, containers, and packaging materials.
Elemental impurities do not have any therapeutic effect and even affect the safety of the drug. For example, some inorganic impurities (cadmium, lead, arsenic, mercury, etc.) produce unknown or harmful pharmacological-toxicological effects even at trace concentration levels, wherein heavy metal impurities tend to accumulate in the body, inactivate proteins, damage human tissue cells, and present a chronic toxicological risk. Some elements (cobalt, copper, etc.) are listed as essential elements for the human body, but at high concentrations they are also harmful to health. Monitoring of elemental impurities plays a crucial role in quality control in pharmaceutical production, controlling their content within acceptable ranges. The existing detection method has limitations, and has the problems of low separation degree, long detection time, low accuracy and the like, so that a general detection method for detecting element impurities in bulk drugs is needed to be established.
Disclosure of Invention
Therefore, aiming at the defects in the prior art, the invention aims to provide a general method for quickly, simply and accurately detecting 10 element impurities in bulk drugs, so as to realize quality control of the bulk drugs and enable the bulk drugs to meet the specified requirements.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a general detection method for 10 element impurities in bulk drugs comprises the following steps:
(1) Preparing a solvent: diluting 68% concentrated nitric acid by 20 times to serve as a solvent for later use;
(2) Preparing a mixed reference stock solution: accurately measuring a proper amount of standard solutions of lithium, vanadium, cobalt, nickel, arsenic, cadmium, antimony, mercury, lead and copper elements, diluting the standard solutions with a solvent to prepare a mixed reference stock solution containing 5 mu g of lithium, 0.2 mu g of vanadium, 0.1 mu g of cobalt, 0.4 mu g of nickel, 0.3 mu g of arsenic, 0.04 mu g of cadmium, 1.8 mu g of antimony, 0.06 mu g of mercury, 0.1 mu g of lead and 6 mu g of copper in each 1ml of standard solution, and shaking up;
(3) Preparing a mixed internal standard stock solution: respectively precisely measuring appropriate amounts of scandium, germanium, indium and bismuth element standard solutions, diluting with a solvent to prepare a mixed internal standard stock solution containing 2 mug of scandium, 2 mug of germanium, 2 mug of indium and 2 mug of bismuth per 1ml, and shaking up;
(4) Preparing a standard curve solution of a reference substance: respectively and precisely measuring 0 mu l, 100 mu l, 200 mu l, 500 mu l, 1ml and 1.5ml of mixed reference stock solution, sequentially placing the mixed reference stock solution into a centrifuge tube, precisely adding 500 mu l of the mixed internal standard stock solution, respectively diluting the mixed internal standard stock solution to 50ml of scales by using a solvent, shaking up to obtain reference standard curve solutions with different concentrations, wherein the concentrations of all elements in the reference standard curve solutions are as follows:
(5) Preparing a test solution: precisely weighing 50-200 mg of fine powder of a sample to be tested, placing the fine powder in a digestion tank, adding 4-8 mL of nitric acid and 1-2 mL of hydrogen peroxide, sealing, and placing the mixture in a microwave digestion instrument for digestion; taking out the digestion tank after complete digestion, placing the digestion tank in an acid dispelling instrument, dispelling acid at 110-160 ℃ until the residual volume is 2mL, cooling, taking out the digestion tank, transferring the digestion instrument into a centrifuge tube, washing the digestion tank with a solvent, combining washing liquids, precisely weighing 1mL of mixed internal standard stock solution, fixing the volume to 50mL scale with the solvent, and shaking up;
(6) Preparing a reagent blank solution: adopting the same operating conditions as the step (5) but not adding a test sample into the digestion tank;
(7) And (3) detection: selecting isotopes of lithium 7, vanadium 51, cobalt 59, nickel 60, copper 63, arsenic 75, cadmium 111, antimony 121, mercury 202 and lead 208, wherein the elements of lithium and vanadium use scandium 45 as internal standard elements, the elements of cobalt, nickel, copper and arsenic use germanium 72 as internal standard elements, the elements of cadmium and antimony use indium 115 as internal standard elements, and the elements of mercury and lead use bismuth 209 as internal standard elements; and (3) respectively injecting the blank solution, the reference substance standard curve solution, the reagent blank solution and the test solution into an inductively coupled plasma mass spectrometer, and recording the response value of each element.
The further improvement is that: the main working parameters of the inductively coupled plasma mass spectrometer in the step (6) are as follows: the detection mode is KED, the radio frequency power is 1400-1550W, the plasma gas flow is 12-14L/min, the carrier gas flow is 0.8-1.0L/min, and the auxiliary gas flow is 0.8-1.0L/min.
The further improvement is that: the digestion conditions in the step (5) are as follows:
| digestion step | Temperature/. Degree.C | Temperature rise time/min | Retention time/min |
| 1 | 120 | 10 | 10 |
| 2 | 150 | 5 | 10 |
| 3 | 180～200 | 10 | 10～60 |
。
By adopting the technical scheme, the invention has the beneficial effects that:
the invention provides a simple, effective and universal detection method aiming at element impurities in raw material medicines, and the detection method can effectively detect elements such as lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead. The average recovery rate of each element is in the range of 86.7-109.3%, which shows that the test method can accurately and quantitatively analyze each element impurity in the bulk drug, and other reagents adopted in the test process cannot interfere with the accuracy of the test result. The RSD of the recovery rate of each element is in the range of 0.93-3.9%, which shows that the test method of the invention has good repeatability and stable test data.
Detailed Description
The following detailed description will be provided for the embodiments of the present invention with reference to specific embodiments, so that how to apply the technical means to solve the technical problems and achieve the technical effects can be fully understood and implemented.
Unless otherwise indicated, the techniques used in the examples are conventional and well known to those skilled in the art, and the reagents and products used are also commercially available. The source, trade name and if necessary the constituents of the reagents used are indicated at the first appearance.
Examples
A general detection method for 10 element impurities in bulk drugs comprises the following steps:
(1) Preparing a solvent: diluting 68% concentrated nitric acid by 20 times to serve as a solvent for later use;
(2) Preparing a mixed reference stock solution: accurately measuring a proper amount of standard solutions of lithium, vanadium, cobalt, nickel, arsenic, cadmium, antimony, mercury, lead and copper elements, diluting the standard solutions with a solvent to prepare a mixed reference stock solution containing 5 mu g of lithium, 0.2 mu g of vanadium, 0.1 mu g of cobalt, 0.4 mu g of nickel, 0.3 mu g of arsenic, 0.04 mu g of cadmium, 1.8 mu g of antimony, 0.06 mu g of mercury, 0.1 mu g of lead and 6 mu g of copper in each 1ml of standard solution, and shaking up;
(3) Preparing a mixed internal standard stock solution: respectively precisely measuring appropriate amounts of scandium, germanium, indium and bismuth element standard solutions, diluting with a solvent to prepare a mixed internal standard stock solution containing 2 mug of scandium, 2 mug of germanium, 2 mug of indium and 2 mug of bismuth per 1ml, and shaking up;
(4) Preparing a standard curve solution of a reference substance: respectively and precisely measuring 0 mu l, 100 mu l, 200 mu l, 500 mu l, 1ml and 1.5ml of mixed reference stock solution, sequentially placing the mixed reference stock solution into a centrifuge tube, precisely adding 500 mu l of the mixed internal standard stock solution, respectively diluting the mixed internal standard stock solution to 50ml of scales by using a solvent, shaking up to obtain reference standard curve solutions with different concentrations, wherein the concentrations of all elements in the reference standard curve solutions are as follows:
(5) Preparing a test solution: accurately weighing 0.1g of fine powder of a sample to be tested, placing the fine powder into a digestion tank, adding 5mL of nitric acid and 1mL of hydrogen peroxide, sealing, placing the digestion tank into a microwave digestion instrument for digestion, wherein the specific digestion conditions are as follows:
taking out the digestion tank after complete digestion, placing the digestion tank in an acid dispelling instrument, dispelling acid at 160 ℃ until the residual volume is 2mL, cooling, taking out the digestion tank, transferring the digestion instrument into a centrifuge tube, washing the digestion tank with a solvent, combining washing liquids, precisely weighing 1mL of mixed internal standard stock solution, fixing the volume to 50mL scale with the solvent, and shaking up;
(6) Preparing a reagent blank solution: adopting the same operating conditions as the step (5) but not adding a test sample into the digestion tank;
(7) Preparing a quality control solution: precisely weighing 0.1g of a sample to be tested, placing the sample in a microwave digestion tank, adding a proper amount of a mixed reference stock solution and 5ml of pure nitric acid, covering and placing the sample for 1h, taking out the sample after digestion, cooling the sample to room temperature, transferring the digestion solution into a centrifuge tube, adding 500 mu l of a mixed internal standard stock solution, metering the volume to 50m l by using a solvent, and shaking up;
(8) And (3) detection: selecting isotopes of lithium 7, vanadium 51, cobalt 59, nickel 60, copper 63, arsenic 75, cadmium 111, antimony 121, mercury 202 and lead 208, wherein the elements of lithium and vanadium use scandium 45 as internal standard elements, the elements of cobalt, nickel, copper and arsenic use germanium 72 as internal standard elements, the elements of cadmium and antimony use indium 115 as internal standard elements, and the elements of mercury and lead use bismuth 209 as internal standard elements; and respectively injecting the blank solution, the reference substance standard curve solution, the reagent blank solution and the sample solution into an inductively coupled plasma mass spectrometer, and recording the response value of each element.
The main working parameters of the inductively coupled plasma mass spectrometer are as follows: the detection mode is KED, the radio frequency power is 1400-1550W, the plasma gas flow is 12-14L/min, the carrier gas flow is 0.8-1.0L/min, and the auxiliary gas flow is 0.8-1.0L/min.
The quality control solution was subjected to a spiking recovery test and the recovery was calculated and the results are shown in table 1.
TABLE 1 System suitability test results
As can be seen from the above table, the average recovery rate of lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead elements in the quality control solution is in the range of 86.2-106.2%, and the actual analysis requirements are met.
The results of the specificity experiments are shown in table 2.
TABLE 2 results of the specificity experiments
From the table, it can be known that the response value ratios of lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury, lead elements and internal standard elements in the solvent and reagent blank solutions are all smaller than the response value ratios of each element and the internal standard element in the linear STD1 solution, which indicates that other reagents in the test method of the present invention do not interfere with the accuracy of the test result.
The mass concentration of each element is used as an abscissa, and the corresponding response value is used as an ordinate to draw a standard curve, the results of linear parameters are shown in table 3, and the results of instrument detection limit and instrument quantitative limit are shown in table 4.
TABLE 3 Linear regression equation, correlation coefficient and Linear Range test results
| Element(s) | Linear equation of equations | Coefficient of correlation r | Linear concentration Range (μ g/L) |
| Lithium ion source | f(x)＝0.0024x+0.0002 | 0.9998 | 0～150 |
| Vanadium oxide | f(x)＝0.1694x+0.0005 | 1.0000 | 0～6.0 |
| Cobalt | f(x)＝0.8412x+0.0005 | 0.9998 | 0～3.0 |
| Nickel (II) | f(x)＝0.2438x+0.0013 | 0.9999 | 0～12.0 |
| Copper (Cu) | f(x)＝0.6179x+0.0504 | 0.9996 | 0～180 |
| Arsenic (As) | f(x)＝0.0236x+0.0003 | 0.9999 | 0～9.0 |
| Cadmium (Cd) | f(x)＝0.0099x+0.0000 | 0.9998 | 0～1.20 |
| Antimony (Sb) | f(x)＝0.0176x+0.0000 | 1.0000 | 0～54.0 |
| Mercury | f(x)＝0.0051x+0.0001 | 1.0000 | 0～1.80 |
| Lead (II) | f(x)＝0.0331x+0.0003 | 0.9999 | 0～3.0 |
As can be seen from the above table, the standard curves of the 10 measured elements have good linear relationship, and the correlation coefficients R are all larger than 0.9995.
TABLE 4 Instrument detection limit and instrument quantification limit results
As can be seen from the table above, the test method of the invention can effectively detect lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead elements.
Accuracy experimental results
Low concentration level accuracy solutions: precisely weighing 0.1g of the product, placing the product in a microwave digestion tank, adding 100 mu l of mixed reference stock solution and 5ml of pure nitric acid, covering the tank, placing the tank for 1h, and digesting according to a digestion program. And taking out the digestion solution after digestion, cooling the digestion solution to room temperature, transferring the digestion solution into a centrifuge tube, adding a proper amount of mixed internal standard stock solution, metering the volume to 50ml by using a solvent, and shaking up to obtain the low-concentration horizontal accuracy solution. In parallel, 3 parts of solution are prepared.
Medium concentration level accuracy solutions: precisely weighing 0.1g of the product, placing the product in a microwave digestion tank, adding 500 mu l of mixed reference stock solution and 5ml of pure nitric acid, covering the tank, placing the tank for 1h, and digesting according to a digestion program. And taking out the digestion solution after digestion, cooling the digestion solution to room temperature, transferring the digestion solution into a centrifuge tube, adding a proper amount of mixed internal standard stock solution, metering the volume to 50ml by using a solvent, and shaking up to obtain the solution with the accuracy of the medium concentration level. In parallel, 3 parts of solution are prepared.
High concentration level accuracy solution: precisely weighing 0.1g of the product, placing the product in a microwave digestion tank, adding 750 mu l of mixed reference stock solution and 5ml of pure nitric acid, covering the tank, placing the tank for 1 hour, and digesting according to a digestion program. Taking out the digestion solution after digestion, cooling the digestion solution to room temperature, transferring the digestion solution to a centrifuge tube, adding a proper amount of mixed internal standard stock solution, fixing the volume to 50ml by using a solvent, and shaking up to obtain the high-concentration horizontal accuracy solution. In parallel, 3 parts of solution are prepared.
Therefore, the background amounts and measured amounts of lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead in the solution with different concentration level accuracy can be calculated, the recovery rate of each element is calculated according to the actual addition amount, and the result is shown in table 5. The specific calculation formula is as follows:
TABLE 5 accuracy test results
From the above table, it can be known that the average recovery rates of lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead in the low, medium and high concentration level accurate solution are in the range of 86.7-109.3%, the RSD of each element recovery rate is in the range of 2.5-4.2%, and each element impurity in the bulk drug can be accurately and quantitatively analyzed.
Results of repeatability experiments
Repetitive solution: precisely weighing 0.1g of the product, placing the product in a microwave digestion tank, adding a proper amount of a mixed reference stock solution and 5ml of pure nitric acid, covering and placing the tank for 1 hour, and digesting according to a digestion program. And taking out the mixture after digestion, cooling the mixture to room temperature, transferring the digestion solution to a centrifuge tube, adding 500 mu l of mixed internal standard stock solution, metering the volume to 50ml by using a solvent, and shaking up the mixture. The test results are shown in Table 6.
TABLE 6 accuracy test results
As can be seen from the table above, the average recovery rates of lithium, vanadium, cobalt, nickel, copper, arsenic, cadmium, antimony, mercury and lead elements in the repetitive solution are in the range of 85.0-107.0%, and the RSD of the recovery rates of the elements is in the range of 0.93-3.9%, which shows that the test method of the invention has good repeatability and stable test data.
The above description is only an embodiment utilizing the technical content of the present disclosure, and any modification and variation made by those skilled in the art can be covered by the claims of the present disclosure, and not limited to the embodiments disclosed.
Claims (3)
1. A general detection method for 10 element impurities in bulk drugs is characterized in that: the method comprises the following steps:
(1) Preparing a solvent: diluting 68% concentrated nitric acid by 20 times to serve as a solvent for later use;
(2) Preparing a mixed reference stock solution: accurately measuring a proper amount of standard solutions of lithium, vanadium, cobalt, nickel, arsenic, cadmium, antimony, mercury, lead and copper elements, diluting the standard solutions with a solvent to prepare a mixed reference stock solution containing 5 mu g of lithium, 0.2 mu g of vanadium, 0.1 mu g of cobalt, 0.4 mu g of nickel, 0.3 mu g of arsenic, 0.04 mu g of cadmium, 1.8 mu g of antimony, 0.06 mu g of mercury, 0.1 mu g of lead and 6 mu g of copper in each 1ml of the mixed reference stock solution, and shaking the mixed reference stock solution uniformly;
(3) Preparing a mixed internal standard stock solution: respectively precisely measuring appropriate amounts of scandium, germanium, indium and bismuth element standard solutions, diluting with a solvent to prepare a mixed internal standard stock solution containing 2 mug of scandium, 2 mug of germanium, 2 mug of indium and 2 mug of bismuth in 1ml, and shaking up;
(4) Preparing a standard curve solution of a reference substance: respectively and precisely measuring 0 mu l, 100 mu l, 200 mu l, 500 mu l, 1ml and 1.5ml of mixed reference stock solution, sequentially placing the mixed reference stock solution into a centrifuge tube, precisely adding 500 mu l of the mixed internal standard stock solution, respectively diluting the mixed internal standard stock solution to 50ml of scales by using a solvent, shaking up to obtain reference standard curve solutions with different concentrations, wherein the concentrations of all elements in the reference standard curve solutions are as follows:
(5) Preparing a test solution: precisely weighing 50-200 mg of fine powder of a sample to be tested, placing the fine powder into a digestion tank, adding 4-8 mL of nitric acid and 1-2 mL of hydrogen peroxide, sealing, and placing the digestion tank into a microwave digestion instrument for digestion; taking out the digestion tank after complete digestion, placing the digestion tank in an acid dispelling instrument, dispelling acid at 110-160 ℃ until the residual volume is 2mL, cooling, taking out the digestion tank, transferring the digestion instrument into a centrifuge tube, washing the digestion tank with a solvent, combining washing liquids, precisely weighing 1mL of mixed internal standard stock solution, fixing the volume to 50mL scale with the solvent, and shaking up;
(6) Preparing a reagent blank solution: adopting the same operating conditions as the step (5) but not adding a test sample into the digestion tank;
(7) And (3) detection: selecting isotopes of lithium 7, vanadium 51, cobalt 59, nickel 60, copper 63, arsenic 75, cadmium 111, antimony 121, mercury 202 and lead 208, wherein the elements of lithium and vanadium use scandium 45 as internal standard elements, the elements of cobalt, nickel, copper and arsenic use germanium 72 as internal standard elements, the elements of cadmium and antimony use indium 115 as internal standard elements, and the elements of mercury and lead use bismuth 209 as internal standard elements; and (3) respectively injecting the solvent, the reference substance standard curve solution, the reagent blank solution and the test substance solution into an inductively coupled plasma mass spectrometer, and recording the response value of each element.
2. The universal detection method for 10 element impurities in bulk drugs according to claim 1, characterized in that: the main working parameters of the inductively coupled plasma mass spectrometer in the step (6) are as follows: the detection mode is KED, the radio frequency power is 1400-1550W, the plasma gas flow is 12-14L/min, the carrier gas flow is 0.8-1.0L/min, and the auxiliary gas flow is 0.8-1.0L/min.
3. The universal detection method for 10 element impurities in bulk drugs according to claim 1, characterized in that: the digestion conditions in the step (5) are as follows:
。
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