CN110487883A - A method of element impurity in detection dutasteride's soft capsule - Google Patents
A method of element impurity in detection dutasteride's soft capsule Download PDFInfo
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Abstract
The invention discloses a kind of methods of element impurity in detection dutasteride's soft capsule.This method includes the following steps: the preparation of (1) sample solution: accurately weighing dutasteride's soft capsule sample, is cleared up in advance to sample, micro-wave digestion, catches up with acid, then cooling, constant volume obtains sample solution；(2) blank solution is prepared；(3) inner mark solution is prepared；(4) standard solution and linear solvent are prepared；(5) it detects and is analyzed with data: carrying out the detection and analysis of element impurity using standard addition method using ICP-MS.Step of the present invention is simple, at low cost, has good measuring accuracy, more extensively, can more effectively control product quality with multielement simultaneous determination.
Description
Technical field
The present invention relates to drug quality detection fields, and in particular to a kind of to detect element impurity in dutasteride's soft capsule
Method.
Background technique
United States Pharmacopeia (USP) announces that the new standard of element impurity in drug was implemented on January 1st, 2018.General rule<232>and
<2232>the day exposure limit (PDE) of list and its permission of concern element is defined based on administration route.This time standard update
Make USP concern element list and PDE in terms of with human drugs registration technology requirement coordination committee (ICH) Q3D fourth stage file
Match.In June, 2016, FDA issued the guideline for covering the element impurity of ICH Q3D in drug.And dutasteride is soft
Capsule should be able to accurately be detected the content of element impurity in the drug by compliance requirement analysis method, to ensure its safety.
7 kinds 1 grade must measured in oral preparation and 2A grades of elements are specified in USP general rule<232>, and soft in dutasteride
It is specific during the production of raw medicine of capsule to joined palladium element.Current most of measuring method can only measure one every time
Element, and some analysis method detection cycles are long, method is complicated for operation, and consumption reagent is also more, cannot fully meet enterprise
Fast and accurately analysis requires.A set of analysis method scientific and effective, that 8 kinds of elemental impurity levels can be measured simultaneously is established, it is right
In more extensively, more effectively control product quality, have important application value.
Summary of the invention
The object of the present invention is to provide a kind of ICP-MS (inductivity coupled plasma mass spectrometry) methods to detect dutasteride's flexible glue
The method of element impurity in capsule more extensively, more effectively controls product quality.
To achieve the object of the present invention, the present invention uses the latest model instrument of platinum Elmer Co., Ltd
2000ICP-MS develops a kind of method that can measure simultaneously 8 kinds of element impurities in the drug, and this method is simple, fast, and energy
Accurate quantification measures the elemental impurity levels of low concentration level, is adopted the technical scheme that: using HNO3, HCl, H2O2, Jin Rong
Liquid clears up dutasteride's soft capsule sample in advance, micro-wave digestion, catches up with after acid, constant volume to obtain sample solution, utilizes ICP-MS (electricity
Feel couple plasma mass spectrometer) using the detection and analysis of standard addition method progress element impurity.
Specifically, the method for the present invention includes following step:
(1) preparation of sample solution: dutasteride's soft capsule sample accurately is weighed, sample is cleared up in advance, microwave disappears
It solves, catch up with acid, then cooling, constant volume obtains sample solution；
(2) blank solution is prepared；
(3) inner mark solution is prepared；
(4) standard solution and linear solvent are prepared；
(5) it detects and is analyzed with data: carrying out the detection and analysis of element impurity using standard addition method using ICP-MS.
In the present invention, in the step (1) sample solution the preparation method comprises the following steps: precision to weigh 0.114g dutasteride soft
Capsule sample, precision pipette 5mL HNO3, 1mL HCl, 1mL H2O2, 1mL gold solution is added in counteracting tank, disappeared in advance
Solution carries out micro-wave digestion after being cooled to room temperature, catching up with acid to liquor capacity after the completion of micro-wave digestion under the conditions of 110 DEG C is 3ml, cold
But it to room temperature, shifts solution into 50ml volumetric flask, repeatedly rinses counteracting tank with ultrapure water, be settled to 50ml, shake up to obtain the final product.
In the present invention, blank solution the preparation method comprises the following steps: precision pipettes 5mL HNO in the step (2)3, 1mL HCl,
1mL H2O2, 1mL gold solution is added in counteracting tank, cleared up in advance, carries out micro-wave digestion, micro-wave digestion after being cooled to room temperature
Catching up with acid to liquor capacity under the conditions of 110 DEG C after the completion is 3ml, is cooled to room temperature, and shifts solution into 50ml volumetric flask, with super
Pure water repeatedly rinses counteracting tank, is settled to 50ml, shakes up to obtain the final product.
In the present invention, in the step (3) inner mark solution the preparation method comprises the following steps: precision pipette 0.35mL internal standard mixing mark
Quasi- solution is settled to scale with diluent to 100mL volumetric flask, and wherein internal standard mixed solution is the nitric acid that mass fraction is 5%,
Wherein the concentration of Bi, Ge, In, Sc, Tb, Y and Li are 10 μ g/mL.
In the present invention, step (4) the Plays solution includes standard solution A, standard solution B, and standard solution A includes
1ppm Cd, 1ppm Pb, 3ppm As, 6ppm Hg, 10ppm Co, 20ppm V, 40ppm Ni, standard solution B include 10ppm
Pd。
In the present invention, in the step (4) linear solvent the preparation method comprises the following steps:
0.25J (std-1) linear solvent: precision pipettes 0.25mL standard solution A, 0.5mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
0.5J (std-2) linear solvent: precision pipettes 0.50mL standard solution A, 1.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
1.0J (std-3) linear solvent: precision pipettes 1.0mL standard solution A, 2.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
1.5J (std-4) linear solvent: precision pipettes 1.5mL standard solution A, 3.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
Wherein, the J is element theory maximum acceptable concentration, as shown in the table:
Preferably, in the present invention, the gold solution the preparation method comprises the following steps: the accurate standard gold solution for pipetting 1000 μ g/mL
1.0mL adds diluent to be settled to 100mL, shakes up to obtain the final product.
Preferably, the present invention in, the diluent the preparation method comprises the following steps: precision pipettes 25.0mL HNO3And 5.0mL
HCl is settled to 500ml with ultrapure water, shakes up to obtain the final product.
Preferably, in the present invention, it is as follows that program is cleared up in advance in the step (1) and (2):
Preferably, in the present invention, micro-wave digestion program is as follows in the step (1) and (2):
| No. | Time/min | Power/W | Temperature/DEG C |
| 1 | 10 | 1600 | 130 |
| 2 | 5 | 1600 | 130 |
| 3 | 20 | 1600 | 180 |
| 4 | 20 | 1600 | 180 |
| 5 | 30 | Natural cooling | Lower than 80 |
In the present invention, the nitric acid refers to that mass fraction is the nitric acid of 67-70%, and hydrogen peroxide refers to that mass fraction is 30-
32% hydrogen peroxide.
The beneficial effects of adopting the technical scheme are that step of the present invention is simple, and it is at low cost, there is good survey
Try precision, ICP-MS detection limit is low, and interference is few, and dynamic linear response range is wide, and analytical precision is high, can with multielement simultaneous determination,
More extensively, product quality is more effectively controlled.
Detailed description of the invention
Fig. 1 is As (arsenic) elemental standards curve；
Fig. 2 is Cd (cadmium) elemental standards curve；
Fig. 3 is Co (cobalt) elemental standards curve；
Fig. 4 is Hg (mercury) elemental standards curve；
Fig. 5 is Ni (nickel) elemental standards curve；
Fig. 6 is Pb (lead) elemental standards curve；
Fig. 7 is Pd (palladium) elemental standards curve；
Fig. 8 is V (vanadium) elemental standards curve；
Fig. 9 is the testing result of element impurity concentration in sample；
Abscissa is concentration (μ g/L) of each element in linear solvent in Fig. 1-8, and ordinate is each element linear molten
The ratio (CPS) of response and internal standard element response in liquid.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.Additional aspect and advantage of the invention will be set forth in part in the description, part
It will become apparent from the description below, or practice through the invention is recognized.It is only used to solve it should be appreciated that being described below
The present invention is released, is not intended to limit the present invention.
Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that covering
Non-exclusionism includes.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those and want
Element, but may include not expressly listed other elements or such composition, step, method, product or device it is intrinsic
Element.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
Indefinite article "an" before element or component of the present invention (goes out the quantitative requirement of element or component with "one"
Occurrence number) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and singular
Element or component also include plural form, unless the quantity obviously only refers to singular.
In addition, term " one embodiment " disclosed below, " some embodiments ", " example ", " specific example " or
The description of " some examples " etc. means that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example include
In at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms are not required
For identical embodiment or example.As long as moreover, technical characteristic involved in each embodiment of the present invention each other it
Between do not constitute conflict and can be combined with each other.
The present invention will be further described in detail below with reference to specific embodiments.
Specifically, the method for the present invention includes following step:
(1) preparation of sample solution: precision weighs 0.114g dutasteride's soft capsule sample, and precision pipettes 5mL HNO3,
1mL HCl, 1mL H2O2, 1mL gold solution is added in counteracting tank, cleared up in advance, micro-wave digestion is carried out after being cooled to room temperature,
Catching up with acid to liquor capacity after the completion of micro-wave digestion under the conditions of 110 DEG C is 3ml, is cooled to room temperature, transfer solution to 50ml capacity
In bottle, repeatedly rinse counteracting tank with ultrapure water, be settled to 50ml, shake up to obtain the final product；
(2) prepare blank solution: precision pipettes 5mL HNO3, 1mL HCl, 1mL H2O2, 1mL gold solution is added to and disappears
It solves in tank, is cleared up in advance, micro-wave digestion is carried out after being cooled to room temperature, catches up with acid after the completion of micro-wave digestion under the conditions of 110 DEG C extremely
Liquor capacity is 3ml, is cooled to room temperature, and shifts solution into 50ml volumetric flask, repeatedly rinses counteracting tank with ultrapure water, be settled to
50ml shakes up to obtain the final product；
(3) prepare inner mark solution: precision pipettes 0.35mL internal standard mixed standard solution to 100mL volumetric flask, uses diluent
It is settled to scale, wherein internal standard mixed solution is the nitric acid that mass fraction is 5%, and wherein Bi, Ge, In, Sc, Tb, Y and Li's is dense
Degree is 10 μ g/mL；
(4) standard solution and linear solvent are prepared, wherein standard solution includes standard solution A, standard solution B, and standard is molten
Liquid A includes 1ppm Cd, 1ppm Pb, 3ppm As, 6ppm Hg, 10ppm Co, 20ppm V, 40ppm Ni, standard solution B packet
Pd containing 10ppm；
(5) it detects and is analyzed with data: carrying out the detection and analysis of element impurity using standard addition method using ICP-MS.
Preferably, to clear up program in advance in the step (1) and (2) as follows:
| No. | Time/min | Temperature/DEG C |
| 1 | 10 | 60 |
| 2 | 30 | 110 |
Preferably, micro-wave digestion program is as follows in the step (1) and (2):
| No. | Time/min | Power/W | Temperature/DEG C |
| 1 | 10 | 1600 | 130 |
| 2 | 5 | 1600 | 130 |
| 3 | 20 | 1600 | 180 |
| 4 | 20 | 1600 | 180 |
| 5 | 30 | Natural cooling | Lower than 80 |
The nitric acid refers to that mass fraction is the nitric acid of 67-70%, and hydrogen peroxide refers to that mass fraction is the double of 30-32%
Oxygen water.
Preferably, in the present invention, the preparation method of the gold solution is the standard gold solution that precision pipettes 1000 μ g/mL
1.0mL adds diluent to be settled to 100mL, shakes up to obtain the final product.
Preferably, the present invention in, the diluent the preparation method comprises the following steps: precision pipettes 25.0mL HNO3And 5.0mL
HCl is settled to 500ml with ultrapure water, shakes up.
Embodiment 1
It calculates maximum to take daily concentration (μ g/g), i.e., element allows maximum to take daily metering (μ g)/dutasteride's soft capsule maximum
Metering (g) is taken daily, the results are shown in Table 1.
1 maximum of table takes daily concentration
Calculating elements theoretical maximum safe level (J) value, unit ppb, calculation formula are as follows:
I.e. maximum takes daily concentration (μ g/g)/dilution because of (mL/g), thus obtains each element J value, as shown in table 2.
2 each element J value of table
Note: dilution gfactor=constant volume/example weight weighs sample 0.114g if pressing one embodiment of the present of invention
It is diluted to 50mL, then dilution gfactor is 439.
Embodiment 2
The preparation of linear solvent and the drafting of elemental standards curve:
0.25J (std-1) linear solvent: precision pipettes 0.25mL standard solution A, 0.5mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
0.5J (std-2) linear solvent: precision pipettes 0.50mL standard solution A, 1.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
1.0J (std-3) linear solvent: precision pipettes 1.0mL standard solution A, 2.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
1.5J (std-4) linear solvent: precision pipettes 1.5mL standard solution A, 3.0mL standard solution B to 50mL capacity
Bottle, diluent are diluted to scale, shake up to obtain the final product；
It is specific as shown in table 3.
3 linear solvent of table
Each element standard curve is as follows, respectively as shown in figures 1-8.
As (arsenic) elemental standards curve: y=0.008x+0.000 (R=0.999920)
Cd (cadmium) elemental standards curve: y=0.045x+0.000 (R=0.999922)
Co (cobalt) elemental standards curve: y=0.325x+0.000 (R=0.999723)
Hg (mercury) elemental standards curve: y=0.018x+0.000 (R=0.999923)
Ni (nickel) elemental standards curve: y=0.094x+0.000 (R=0.999892)
Pb (lead) elemental standards curve: y=0.120x+0.000 (R=0.999665)
Pd (palladium) elemental standards curve: y=0.247x+0.000 (R=0.997179)
V (vanadium) elemental standards curve: y=0.096x+0.000 (R=0.999715)
Embodiment 3
Precision weighs 0.114g dutasteride's soft capsule sample, and precision pipettes 5mL HNO3, 1mL HCl, 1mL H2O2,
1mL gold solution, is added in counteracting tank, is cleared up in advance, carries out micro-wave digestion after being cooled to room temperature, after the completion of micro-wave digestion in
It is 3ml that acid to liquor capacity is caught up under the conditions of 110 DEG C, is cooled to room temperature, and shifts solution into 50ml volumetric flask, multiple with ultrapure water
Counteracting tank is rinsed, 50ml is settled to, shakes up up to sample solution, uses ICP-MS (inductively coupled plasma constitution of the invention
Spectrum) method detection dutasteride's soft capsule in element impurity.
Element impurity concentration (μ g/g)=C*Dilution Factor*10 in sample-3, wherein C is concentration of element (μ g/
L), Dilution Factor is dilution gfactor, i.e. constant volume/example weight, unit mL/g, testing result such as Fig. 9 institute
Show.
Wherein, Conc. indicates instrument detection gained concentration, by sample detection typical case map it is found that 8 kinds of element impurities
Concentration it is lower, the results are shown in Table 4.
Concentration of element in 4 sample of table
| Element term | Instrument detectable concentration | Concentration of element in sample |
| Pb (lead) | 0.1111ppb=0.1111 μ g/L | 0.1111μg/L*50ml/0.114g*10-3=0.049 μ g/g |
| Hg (mercury) | 0.0346ppb=0.0346 μ g/L | 0.0346μg/L*50ml/0.114g*10-3=0.015 μ g/g |
| Cd (cadmium) | - 0.0011ppb=0 μ g/L | 0μg/L*50ml/0.114g*10-3=0 μ g/g |
| As (arsenic) | - 0.0228ppb=0 μ g/L | 0μg/L*50ml/0.114g*10-3=0 μ g/g |
| Co (cobalt) | 0.0117ppb=0.0117 μ g/L | 0.0117μg/L*50ml/0.114g*10-3=0.005 μ g/g |
| V (vanadium) | - 0.0351ppb=0 μ g/L | 0μg/L*50ml/0.114g*10-3=0 μ g/g |
| Ni (nickel) | 0.2295ppb=0.2295 μ g/L | 0.2295μg/L*50ml/0.114g*10-3=0.101 μ g/g |
| Pd (palladium) | 0.0125ppb=0.0125 μ g/L | 0.0125μg/L*50ml/0.114g*10-3=0.005 μ g/g |
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of method of element impurity in detection dutasteride's soft capsule, which is characterized in that this method includes the following steps:
(1) preparation of sample solution: dutasteride's soft capsule sample accurately is weighed, sample is cleared up in advance, micro-wave digestion, is caught up with
Acid, then cooling, constant volume, obtains sample solution；
(2) blank solution is prepared；
(3) inner mark solution is prepared；
(4) standard solution and linear solvent are prepared；
(5) it detects and is analyzed with data: carrying out the detection and analysis of element impurity using standard addition method using ICP-MS.
2. the method for element impurity in detection dutasteride's soft capsule according to claim 1, which is characterized in that the step
Suddenly in (1) sample solution the preparation method comprises the following steps: precision weighs 0.114g dutasteride's soft capsule sample, precision pipettes 5mL
HNO3, 1mL HCl, 1mL H2O2, 1mL gold solution is added in counteracting tank, cleared up in advance, carries out microwave after being cooled to room temperature
Resolution, it is 3ml that micro-wave digestion catches up with acid to liquor capacity under the conditions of 110 DEG C after the completion, is cooled to room temperature, transfer solution to 50ml
In volumetric flask, repeatedly rinse counteracting tank with ultrapure water, be settled to 50ml, shake up to obtain the final product.
3. the method for element impurity in detection dutasteride's soft capsule according to claim 1, which is characterized in that the step
Suddenly in (2) blank solution the preparation method comprises the following steps: precision pipettes 5mL HNO3, 1mL HCl, 1mL H2O2, 1mL gold solution is added to
It in counteracting tank, is cleared up in advance, micro-wave digestion is carried out after being cooled to room temperature, catches up with acid under the conditions of 110 DEG C after the completion of micro-wave digestion
It is 3ml to liquor capacity, is cooled to room temperature, shifts solution into 50ml volumetric flask, repeatedly rinse counteracting tank, constant volume with ultrapure water
To 50ml, shake up to obtain the final product.
4. the method for element impurity in detection dutasteride's soft capsule according to claim 1, which is characterized in that the step
Suddenly in (3) inner mark solution the preparation method comprises the following steps: precision pipettes 0.35mL internal standard mixed standard solution to 100mL volumetric flask, use is dilute
It releases agent and is settled to scale, wherein internal standard mixed solution is the nitric acid that mass fraction is 5%, wherein Bi, Ge, In, Sc, Tb, Y and Li
Concentration be 10 μ g/mL.
5. the method for element impurity in detection dutasteride's soft capsule according to claim 1, which is characterized in that the step
Suddenly (4) Plays solution includes standard solution A, standard solution B, and standard solution A includes 1ppm Cd, 1ppm Pb, 3ppm As,
6ppm Hg, 10ppm Co, 20ppm V, 40ppm Ni, standard solution B include 10ppm Pd.
6. the method for element impurity in detection dutasteride's soft capsule according to claim 1, which is characterized in that the step
Suddenly in (4) linear solvent the preparation method comprises the following steps:
0.25J linear solvent: precision pipettes 0.25mL standard solution A, 0.5mL standard solution B to 50mL volumetric flask, and diluent is dilute
It releases to scale, shakes up to obtain the final product；
0.5J linear solvent: precision pipettes 0.50mL standard solution A, 1.0mL standard solution B to 50mL volumetric flask, and diluent is dilute
It releases to scale, shakes up to obtain the final product；
1.0J linear solvent: precision pipettes 1.0mL standard solution A, 2.0mL standard solution B to 50mL volumetric flask, dilutes dilution agent
To scale, shake up to obtain the final product；
1.5J linear solvent: precision pipettes 1.5mL standard solution A, 3.0mL standard solution B to 50mL volumetric flask, dilutes dilution agent
To scale, shake up to obtain the final product；
Wherein, the J is element theory maximum acceptable concentration, as shown in the table:
7. according to the method for element impurity in the described in any item detection dutasteride's soft capsules of claim 2 and 3, feature exists
In, the gold solution the preparation method comprises the following steps: the accurate standard gold solution 1.0mL for pipetting 1000 μ g/mL, adds diluent to be settled to
100mL shakes up to obtain the final product.
8. according to the method for element impurity in the described in any item detection dutasteride's soft capsules of claim 6-7, feature exists
In, the diluent the preparation method comprises the following steps: precision pipettes 25.0mL HNO3With 5.0mL HCl, it is settled to 500ml with ultrapure water,
It shakes up to obtain the final product.
9. according to the method for element impurity in the described in any item detection dutasteride's soft capsules of claim 2 and 3, feature exists
In it is as follows to clear up program in advance in the step (1) and (2):
10. according to the method for element impurity in the described in any item detection dutasteride's soft capsules of claim 2 and 3, feature
It is, micro-wave digestion program is as follows in the step (1) and (2):
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Cited By (3)
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| CN111678972A (en) * | 2020-06-19 | 2020-09-18 | 广州汇标检测技术中心 | Method for detecting impurity elements in bulk drugs |
| CN113567537A (en) * | 2021-07-15 | 2021-10-29 | 人福普克药业（武汉）有限公司 | Method for determining element impurities in OTC soft capsules by using inductively coupled plasma mass spectrometry technology |
| CN114487079A (en) * | 2021-12-31 | 2022-05-13 | 乳源东阳光药业有限公司 | Analysis method for measuring elemental impurity silver in rosuvastatin calcium by ICP-MS |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111678972A (en) * | 2020-06-19 | 2020-09-18 | 广州汇标检测技术中心 | Method for detecting impurity elements in bulk drugs |
| CN113567537A (en) * | 2021-07-15 | 2021-10-29 | 人福普克药业（武汉）有限公司 | Method for determining element impurities in OTC soft capsules by using inductively coupled plasma mass spectrometry technology |
| CN114487079A (en) * | 2021-12-31 | 2022-05-13 | 乳源东阳光药业有限公司 | Analysis method for measuring elemental impurity silver in rosuvastatin calcium by ICP-MS |
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