CN109632934A - A kind of analysis method of sufentanil citrate and production system compatibility - Google Patents
A kind of analysis method of sufentanil citrate and production system compatibility Download PDFInfo
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- G—PHYSICS
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- G—PHYSICS
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Abstract
The present invention relates to element technology analysis fields in drug, and in particular to a kind of analysis method of sufentanil citrate and production system compatibility.The present invention relates to the analysis methods of a kind of sufentanil citrate and production system compatibility, the element of detection includes 20 kinds of elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo, W, the following steps are included: (1) sample treatment: after sufentanil citrate is dissolved in water by S1., pH is adjusted with 1% citric acid soln, it is settled to 2L with ultrapure water, obtains sample mother liquor；S2. it takes 500 μ L of sample mother liquor in 50mL volumetric flask, is diluted to scale with diluent to get sample solution.(2) standard solution is prepared；(3) inner mark solution is prepared；(4) ICP-MS is tested: sample solution, standard solution, inner mark solution being tested by ICP-MS, obtain the content of each element.
Description
Technical field
The present invention relates to element technology analysis fields in drug, and in particular to a kind of sufentanil citrate and production system
The analysis method of compatibility.
Background technique
Sufentanil, it is clinical it is medicinal be its citrate, i.e. sufentanil citrate, its chemical name is
propanamide,N-[4-(methoxymethyl)-1-[2-(2-thienyl)ethyl]-4-piperidinyl]-N-
Phenyl-2-hydroxy-1,2,3-propanetricarboxylate, molecular formula C22H30N2O2S·C6H8O7.Molecular weight
578.66.Nineteen eighty-three lists in Holland for the first time, and character is white crystals or crystalline powder.Soluble easily in water, ethyl alcohol, does not dissolve in
Chloroform, ether.Sufentanil citrate is used as antalgesic.It is interior as analgestic in holding time for balanced anesthesia.?
As anesthetic when the induction and maintenance of anesthesia.
State's food medicine prison infuses [2011] No. 430 file distributions and carries out the drug standards about subsidy from central government finance in 2011 is carried out
The notice of revision proposes requirement to the raising work of 957 drug standards, wherein just including that sufentanil citrate is infused
Penetrate liquid.
The work of fentanyl citrate injection quality standard is improved, key is to improve fentanyl citrate process liquid
Quality standard.The study found that improve the quality standard of sufentanil citrate process liquid, sufentanil citrate is controlled
Constituent content is particularly critical in process liquid.
Summary of the invention
In order to solve the above-mentioned technical problem, the first aspect of the invention provides a kind of sufentanil citrate and production
The analysis method of system compatibility, the element of detection include As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li,
20 kinds of elements of Ni, Pb, Sb, V, Mo, W, comprising the following steps:
(1) sample treatment
S1. after sufentanil citrate being dissolved in water, pH is adjusted with 1% citric acid soln, 2L is settled to ultrapure water, obtains
To sample mother liquor；
S2. it takes 500 μ L of sample mother liquor in 50mL volumetric flask, is diluted to scale with diluent to get sample solution；
(2) standard solution is prepared；
(3) inner mark solution is prepared；
(4) ICP-MS is tested: sample solution, standard solution, inner mark solution being tested by ICP-MS, obtain each member
The content of element.
As a kind of perferred technical scheme, adjusting pH with 1% citric acid soln in the step S1 is 3.7~4.2.
As a kind of perferred technical scheme, adjusting pH with 1% citric acid soln in the step S1 is 3.8.
As a kind of perferred technical scheme, diluent is concentrated nitric acid, hydrochloric acid and 0.1% paregal O-in the step S2
10 mixed solution.
As a kind of perferred technical scheme, the volume ratio of the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10 are as follows: (6
~10): (0.5~2): 1.
As a kind of perferred technical scheme, the volume ratio of the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10 are as follows: 8:
2:1.
As a kind of perferred technical scheme, the internal standard element of inner mark solution is Sc, Y and Bi in the step (3).
As a kind of perferred technical scheme, in the inner mark solution, the concentration of Sc, Y and Bi are respectively 50~150 μ
g/L。
As a kind of perferred technical scheme, ICP-MS determination condition in the step (4): radio-frequency generator output power
For 1400~1600W；Plasma gas flow velocity is 15~20L/min；Secondary air speed is 1.0~1.4L/min；Atomization air flow
Speed is 0.85L/min.
As a kind of perferred technical scheme, the plasma gas and auxiliary gas are respectively argon gas and/or helium.
The utility model has the advantages that this method has good accuracy, it can be used as test method and carrying out sufentanil citrate
The measurement of 20 kinds of elements in process liquid.The result shows that: the analysis method object element is linearly good, detection limit, accuracy
Meet measurement to require；The method of the present invention has the advantages such as easy to operate, analysis time is short, stabilization is accurate simultaneously.
Specific embodiment
For the purpose of following detailed description, it should be understood that the present invention can be used various substitutions variation and step it is suitable
Sequence, unless specifically stated on the contrary.In addition, being indicated in the case where in addition in any operational instances or otherwise pointing out
Such as all numbers of the amount of ingredient used in description and claims should be understood in all cases by term
" about " it modifies.Therefore, unless indicated to the contrary, the numerical parameter otherwise illustrated in the following description and appended dependent claims is root
The approximation changed according to the expected performance of the invention to be obtained.It is at least not intended to for the applicable of doctrine of equivalents being limited in
In the scope of the claims, each numerical parameter should at least be given up according to the number of the effective digital of report and by the way that application is common
Enter technology to explain.
Although illustrating that broad range of numberical range and parameter of the invention are approximations, listed in specific example
Numerical value is reported as accurately as possible.However, any numerical value inherently includes the standard deviation by finding in its each self-test measurement
The certain errors necessarily led to.
When a numberical range disclosed herein, above range is considered as continuously, and the minimum value including the range and most
Big value and each value between this minimum value and maximum value.Further, when range refers to integer, including the model
Each integer between minimum value and maximum value enclosed.In addition, when providing multiple range Expressive Features or characteristic, Ke Yihe
And the range.In other words, unless otherwise specified, otherwise all ranges disclosed herein are understood to include and are wherein included into
Any and all subrange.For example, should be regarded as including between minimum value 1 and maximum value 10 from the specified range of " 1 to 10 "
Any and all subrange.The Exemplary range of range 1 to 10 include but is not limited to 1 to 6.1,3.5 to 7.8,5.5 to
10 etc..
To solve the above-mentioned problems, the present invention provides the analyses of a kind of sufentanil citrate and production system compatibility
Method, the element of detection include As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo, W
20 kinds of elements, comprising the following steps:
(1) sample treatment
S1. after sufentanil citrate being dissolved in water, pH is adjusted with 1wt% citric acid soln, is settled to 2L with ultrapure water,
Obtain sample mother liquor；
S2. it takes 500 μ L of sample mother liquor in 50mL volumetric flask, is diluted to scale with diluent to get sample solution.
(2) standard solution is prepared
(3) inner mark solution is prepared
(4) ICP-MS is tested: sample solution, standard solution, inner mark solution being tested by ICP-MS, obtain each member
The content of element.
Wherein: the preparation of 1% citric acid soln: weighing 200mg citric acid, is settled to 20ml with ultrapure water to obtain the final product.
Sample treatment
As a kind of perferred technical scheme, the quality of sufentanil citrate is 75~300mg in the step S1.
Preferably, the quality of sufentanil citrate is 150mg in the step S1.
As a preferred embodiment, adjusting pH with 1% citric acid soln in the step S1 is 3.7~4.2.
20 kinds of elements in sufentanil citrate process liquid are measured, discovery is more accurate using citric acid test result,
So that the rate of recovery, rate of recovery RSD are excellent in, inventor speculates the possible reason is using citron acid dissolution citric acid Shu Fen
Too Buddhist nun weakens matrix effect, and preferable to the dissolubility of drug using 1% citric acid soln first is that exogenous impurity will not be introduced,
And by adjusting PH be 3.7~4.2, drug can sufficiently be dissolved with this condition and is not easily decomposed or oxidation deterioration, be avoided that
It surveys element to be stain, improves test accuracy；Second is that since the presence of citric acid can improve carbon and carbon containing mostly original in plasma
The density of daughter ion, the higher element of ionization potential can be by its electronics transfer to carbon and carbon containing multi-atomic ion, and then improves
The degree of ionization of the higher Partial Elements of ionization energy in the plasma.
As a preferred embodiment, adjusting pH with 1% citric acid soln in the step S1 is 3.8.
As a preferred embodiment, diluent is concentrated nitric acid, hydrochloric acid and 0.1% paregal O-in the step S2
10 mixed solution.
As a preferred embodiment, the volume ratio of the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10 are as follows: (6
~10): (0.5~2): 1.
As a preferred embodiment, the volume ratio of the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10 are as follows: 8:
2:1.
Wherein, the concentrated nitric acid refers to that mass fraction is 68% nitric acid.
The paregal O -10 refers to fatty alcohol polyoxyethylene ether, and the purchase of paregal O -10 is in Jiangsu Province Hai'an petroleum
Work.
The preparation of 0.1% paregal O -10: taking the paregal O -10 of 100mg, is settled to 100mL with ultrapure water, i.e.,
?.
Inventor has found that nitric acid can prevent small metal oxide particle from generating in the course of the study, makes metal molten
It is in free state in liquid, but citric acid presence can generate certain resistance to it, so single use metal dissolving is incomplete, and a
Other metallic element easily forms precipitating in diluent, therefore is compounded with nitric acid using hydrochloric acid, make the result of extraction of sample into
One step improves, but since the presence of hydrochloric acid will lead to the interference of polyion atom, so a certain amount of 0.1% is added in diluent
Paregal O -10 dissolves, and when the volume ratio of concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10 is 8:2:1, diluent and citron
Acid interaction can effectively change intermolecular interaction and aerosol particle size etc., so that analyte enters plasma
Transmission rate in body increases, and improves nebulization efficiency, so as to improve analysis performance, so that it is minimum to the interference of matrix, from
And keeping detection line lower, measurement result is more accurate.
Standard solution is prepared
As a preferred embodiment, the preparation steps of the standard solution are as follows:
It is appropriate to draw elemental standards mother liquor, is diluted respectively with diluent to obtain the final product, wherein in prepared standard solution:
V, the concentration of each element of Co, Ni, As, Cd, Sb, Pb is respectively 0.1,0.5,1,2,5 μ g/L.
The concentration of Hg element is 0.1,0.5,1,1.5,2 μ g/L.
The concentration of each element of Li, B, Al, Cr, Mn, Cu, Ba is respectively 10,20,50,100,200 μ g/L.
The concentration of each element of Si, Fe, Zn is respectively 100,200,500,1000,2000 μ g/L.
Wherein, the diluent concrete component and parts by weight of the standard solution are the same as step S2.
Preferably, the preparation concrete operations of the standard solution are as follows:
(1) 50 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 50 μ L, 3 element hybrid standard mother liquor, 50 μ is added
L, 15 element hybrid standard mother liquor, 50 μ L, is diluted to scale with diluent, shakes up to obtain the final product.Wherein, As, Cd, Co, Ni, Pb, Sb,
V, it is 10 μ g/L, Fe, Zn, Si members that Hg, Mo, W concentration of element, which are 0.1 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn concentration of element,
Plain concentration is 100 μ g/L.
(2) 250 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 250 μ L, 3 element hybrid standard mother liquors is added
250 μ L, 15 element hybrid standard mother liquor, 100 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein, As, Cd, Co, Ni,
Pb, Sb, V, Hg, Mo, W concentration of element are that 0.5 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element spiked levels are 20 μ g/L,
Fe, Zn, Si element spiked levels are 200 μ g/L.
(3) 500 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 500 μ L, 3 element hybrid standard mother liquors is added
500 μ L, 15 element hybrid standard mother liquor, 250 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein, As, Cd, Co, Ni,
Pb, Sb, V, Hg, Mo, W concentration of element are that 1 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element spiked levels are 50 μ g/L,
Fe, Zn, Si element spiked levels are 500 μ g/L.
(4) 750 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 1000 μ L, 3 element hybrid standard mother liquors is added
1000 μ L, 15 element hybrid standard mother liquor, 500 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein, As, Cd, Co, Ni,
Pb, Sb, V, Mo, W concentration of element are that 2 μ g/L, Hg concentration of element are 1.5 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element mark-ons
Concentration is that 100 μ g/L, Fe, Zn, Si element spiked levels are 1000 μ g/L.
(5) 1000 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 2500 μ L, 3 element hybrid standard mother liquors is added
2500 μ L, 15 element hybrid standard mother liquor, 1000 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein, As, Cd, Co, Ni,
Pb, Sb, V, Mo, W concentration of element are that 5 μ g/L, Hg concentration of element are that 2 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element mark-ons are dense
Degree is that 200 μ g/L, Fe, Zn, Si element spiked levels are 2000 μ g/L.
Wherein, Hg elemental standards mother liquor, 7 element hybrid standard mother liquors, 3 element hybrid standard mother liquors, 15 elements mixing mark
The specifying information of quasi- mother liquor is shown in Table 1.
Table 1
Inner mark solution is prepared
As a preferred embodiment, the internal standard element of inner mark solution is Sc, Y and Bi in the step (3).
As a preferred embodiment, the preparation concrete operation step of the inner mark solution are as follows:
It is appropriate to draw Sc, Y and Bi element internal standard stock solution that concentration is 1000mg/L, is diluted to diluent certain dense
Degree.
As a preferred embodiment, the concentration of Sc, Y and Bi are 80~120 μ g/L in the inner mark solution.
Preferably, in the inner mark solution, the concentration of Sc, Y and Bi are 100 μ g/L.
Inventor 20 kinds of elements in sample are tested (As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg,
Li, Ni, Pb, Sb, V, Mo, W), discovery, which selects tri- kinds of elements of Sc, Y, Bi as internal standard, can make test result more accurate, send out
Bright people is presumably due to sample to be tested itself and does not contain three kinds of elements, and the mass number of three and the first ionization energy and quilt
It surveys element to be close, reduces matrix effect；Furthermore the response of internal standard element is easy to be influenced by matrix, citric acid in matrix
The variation of content will cause the biggish fluctuation of internal standard, matrix sample is subjected to appropriate acidification dilution, adjust citron acid content with
And suitable internal standard can effectively reduce matrix effect and sour depression effect, it is ensured that the stabilization and accuracy of test result.
The diluent concrete component and parts by weight of the inner mark solution are the same as step S2.
ICP-MS test
As a preferred embodiment, ICP-MS determination condition in the step (4): radio-frequency generator output power
For 1400~1600W；Plasma gas flow velocity is 15~20L/min；Secondary air speed is 1.0~1.4L/min；Atomization air flow
Speed is 0.85L/min.
Preferably, ICP-MS determination condition in the step (4): radio-frequency generator output power is 1500W；Plasma (orifice) gas
Body flow velocity is 16L/min；Secondary air speed is 1.1L/min；Atomization gas flow velocity is 0.85L/min.
As a preferred embodiment, the plasma gas and auxiliary gas are respectively argon gas and/or helium.
Preferably, the plasma gas and auxiliary gas are respectively argon gas.
As a preferred embodiment, described internal standard element Sc, Y, Bi are introduced online by T-type sampling valve.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
The some nonessential modifications and adaptations made according to the content of aforementioned present invention, still fall within protection scope of the present invention.
In addition, if without other explanations, it is raw materials used to be all commercially available.
Embodiment
Embodiment 1
A kind of analysis method of sufentanil citrate and production system compatibility, the element of detection include As, Cd, B,
20 kinds of elements of Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo, W, comprising the following steps:
(1) sample treatment
S1. after 150mg sufentanil citrate being dissolved in water, adjusting pH with 1% citric acid soln is 3.7, uses ultrapure water
It is settled to 2L, obtains sample mother liquor；
S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with the volume of concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10
Scale is diluted to than the diluent for 6:0.5:1 to get sample solution.
(2) standard solution is prepared
The preparation concrete operations of the standard solution are as follows:
(1) 50mL volumetric flask is taken, it is mixed that 50 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 50 μ L, 3 elements are added
50 μ L of standardization mother liquor, 15 element hybrid standard mother liquor, 50 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein, As, Cd,
Co, Ni, Pb, Sb, V, Hg, Mo, W concentration of element are that 0.1 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element spiked levels are
10 μ g/L, Fe, Zn, Si element spiked levels are 100 μ g/L.
(2) 50mL volumetric flask is taken, 250 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 250 μ L, 3 elements is added
250 μ L of hybrid standard mother liquor, 15 element hybrid standard mother liquor, 100 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein,
As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo, W concentration of element are that 0.5 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element mark-on is dense
Degree is that 20 μ g/L, Fe, Zn, Si element spiked levels are 200 μ g/L.
(3) 50mL volumetric flask is taken, 500 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 500 μ L, 3 elements is added
500 μ L of hybrid standard mother liquor, 15 element hybrid standard mother liquor, 250 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein,
As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo, W concentration of element are 1 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn element spiked levels
It is 50 μ g/L, Fe, Zn, Si element spiked levels is 500 μ g/L.
(4) 50mL volumetric flask is taken, 750 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 1000 μ L, 3 elements is added
1000 μ L of hybrid standard mother liquor, 15 element hybrid standard mother liquor, 500 μ L, are diluted to scale with diluent, shake up to obtain the final product.Wherein,
As, Cd, Co, Ni, Pb, Sb, V, Mo, W concentration of element be 2 μ g/L, Hg concentration of element be 1.5 μ g/L, Al, B, Ba, Cr, Cu,
Li, Mn element spiked levels are that 100 μ g/L, Fe, Zn, Si element spiked levels are 1000 μ g/L.
(5) 50mL volumetric flask is taken, 1000 μ L of Hg elemental standards mother liquor, 7 element hybrid standard mother liquor, 2500 μ L, 3 yuan is added
Plain 2500 μ L of hybrid standard mother liquor, 15 element hybrid standard mother liquor, 1000 μ L, are diluted to scale with diluent, shake up to obtain the final product.Its
In, As, Cd, Co, Ni, Pb, Sb, V, Mo, W concentration of element be 5 μ g/L, Hg concentration of element be 2 μ g/L, Al, B, Ba, Cr, Cu,
Li, Mn element spiked levels are that 200 μ g/L, Fe, Zn, Si element spiked levels are 2000 μ g/L.
Wherein, the diluent concrete component and parts by weight of the standard solution are the same as step S2.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
(3) inner mark solution is prepared
The preparation concrete operations of the inner mark solution are as follows:
Absorption concentration is that Sc, Y and Bi element internal standard stock solution of 1000mg/L is appropriate, is diluted to diluent certain dense
It spends to obtain the final product.
Wherein, in the inner mark solution, the concentration of Sc, Y and Bi are 100 μ g/L.
The diluent concrete component and parts by weight of the inner mark solution are the same as step S2.
(4) ICP-MS is tested: sample solution, standard solution, inner mark solution being tested by ICP-MS, obtain each member
The content of element.
Wherein, ICP-MS determination condition: radio-frequency generator output power is 1500W；Plasma gas flow velocity is 16L/
min；Secondary air speed is 1.1L/min；Atomization gas flow velocity is 0.85L/min.
The plasma gas and auxiliary gas are respectively argon gas.
Embodiment 2
A kind of analysis method of sufentanil citrate and production system compatibility, the specific steps are the same as those in embodiment 1, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 4.2, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 6:0.5:1 is diluted to scale to get sample solution.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
Embodiment 3
A kind of analysis method of sufentanil citrate and production system compatibility, the specific steps are the same as those in embodiment 1, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 6:0.5:1 is diluted to scale to get sample solution.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
Embodiment 4
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 3, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 6:2:1 is diluted to scale to get sample solution.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
Embodiment 5
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 3, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 10:2:1 is diluted to scale to get sample solution.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
Embodiment 6
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 3, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 8:2:1 is diluted to scale to get sample solution.
To standard solution, sample introduction is analyzed, and using concentration as abscissa, peak area is ordinate, and instrument calculates recurrence side automatically
Journey obtains linearly dependent coefficient R greater than 0.999.
Comparative example 1
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 6, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 2.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 8:2:1 is diluted to scale to get sample solution.
Comparative example 2
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 6, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 5.0, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and 0.1% paregal O -10 is that the diluent of 8:2:1 is diluted to scale to get sample solution.
Comparative example 3
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 6, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
Acid, the diluent that the volume ratio of hydrochloric acid is 8:3 are diluted to scale to get sample solution.
Comparative example 4
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 7, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
Acid, the diluent that the volume ratio of 0.1% paregal O -10 is 8:3 are diluted to scale to get sample solution.
Comparative example 5
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 7, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and peregal O-15 is that the diluent of 8:2:1 is diluted to scale to get sample solution.
The purchase of paregal O -15 is in Jiangsu Province Hai'an petrochemical industry.
Comparative example 6
A kind of analysis method of sufentanil citrate and production system compatibility, specific steps are the same as embodiment 7, difference
It is: the method for sample treatment are as follows: after 150mg sufentanil citrate is dissolved in water by S1., adjust pH with 1% citric acid soln
It is 3.8, is settled to 2L with ultrapure water, obtains sample mother liquor；S2. take 500 μ L of sample mother liquor in 50mL volumetric flask, with dense nitre
The volume ratio of acid, hydrochloric acid and peregal O-8 is that the diluent of 8:2:1 is diluted to scale to get sample solution.
The purchase of paregal O -8 is in Jiangsu Province Hai'an petrochemical industry.
Performance Evaluation
Measure embodiment and the accuracy of comparative example detection method, specificity, precision-repeatability.Wherein embodiment 6
Experimental result is shown in Table 2, in accuracy test RSD be three groups of data measure as a result, only putting one group of rate of recovery in table.
(1) accuracy detects:
Prepare that the horizontal solution of low concentration, middle concentration level solution, sample introduction is analyzed for the horizontal solution of high concentration, calculate the rate of recovery and
The rate of recovery relative standard deviation RSD, unit %.
Low concentration is horizontal: taking 500 μ L of sample mother liquor in 50mL volumetric flask, 50 μ L of Hg elemental standards mother liquor, 7 elements is added
50 μ L of hybrid standard mother liquor, 3 element hybrid standard mother liquor, 50 μ L, 15 element hybrid standard mother liquor, 50 μ L, are diluted to diluent
Scale shakes up to obtain the final product.Wherein, As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo, W concentration of element be 0.1 μ g/L, Al, B, Ba, Cr,
Cu, Li, Mn concentration of element are that 10 μ g/L, Fe, Zn, Si concentration of element are 100 μ g/L.Prepare 3 parts of solution in parallel with method.
Middle concentration level: taking 500 μ L of sample mother liquor in 50mL volumetric flask, addition 500 μ L of Hg element hybrid standard mother liquor,
7 element hybrid standard mother liquor, 500 μ L, 3 element hybrid standard mother liquor, 500 μ L, 15 element hybrid standard mother liquor, 250 μ L, with dilution
Dilution agent shakes up to scale to obtain the final product.Wherein, As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo, W concentration of element be 1 μ g/L, Al, B,
Ba, Cr, Cu, Li, Mn concentration of element are that 50 μ g/L, Fe, Zn, Si concentration of element are 500 μ g/L.Prepare 3 parts of solution in parallel with method.
High concentration is horizontal: take 500 μ L of sample mother liquor in 50mL volumetric flask, addition 750 μ L of Hg element hybrid standard mother liquor,
7 element hybrid standard mother liquor, 1000 μ L, 3 element hybrid standard mother liquor, 1000 μ L, 15 element hybrid standard mother liquor, 500 μ L, use are dilute
Dilution agent is released to scale, is shaken up to obtain the final product.Wherein, As, Cd, Co, Ni, Pb, Sb, V element concentration are that 2 μ g/L, Hg concentration of element are
1.5 μ g/L, Al, B, Ba, Cr, Cu, Li, Mn concentration of element are that 100 μ g/L, Fe, Zn, Si concentration of element are 1000 μ g/L.Same method
3 parts of solution of preparation in parallel.
(2) specificity detects: the accuracy solution of process white solution, sample solution and middle concentration level being taken to distinguish sample introduction
Analysis calculates RSD, unit %.
Process white solution is prepared: 500 μ L are in 50mL volumetric flask for water intaking, are diluted to scale with diluent, shake up to obtain the final product.
(3) precision-repeatability detection: preparing repeated solution, sample introduction is analyzed, calculates RSD, unit %.
Repeated solution is prepared: taking 500 μ L of sample mother liquor in 50mL volumetric flask, Hg element hybrid standard mother liquor is added
500 μ L, 7 element hybrid standard mother liquor, 500 μ L, 3 element hybrid standard mother liquor, 500 μ L, 15 element hybrid standard mother liquor, 250 μ L,
It is diluted to scale with diluent, shakes up to obtain the final product.Wherein, As, Cd, Co, Ni, Sb, Pb, V, Hg, Mo, W element spiked levels are 1 μ
G/L, Al, B, Ba, Cr, Cu, Li, Mn element spiked levels are that 50 μ g/L, Fe, Zn, Si element spiked levels are 500 μ g/L.Together
Method prepares 6 parts of solution in parallel.
Wherein, the diluent of solution is prepared with each embodiment.
2 embodiment of table, 6 test result
Measure Examples 1 to 5 and the accuracy (low concentration is horizontal) of 1~6 detection method of comparative example, specificity, precision-
Repeatability detection.Wherein, using V element as representative, the data of V element such as table 3.
3 V element test result of table
The above described is only a preferred embodiment of the present invention, be not the limitation for making other forms to invention, it is any
Those skilled in the art are changed or are changed to the equivalent of equivalent variations possibly also with the technology contents of the disclosure above
Embodiment, but without departing from the technical solutions of the present invention, above embodiments are made according to the technical essence of the invention
Any simple modification, equivalent variations and remodeling, still fall within the protection scope of technical solution of the present invention.
Claims (10)
1. the analysis method of a kind of sufentanil citrate and production system compatibility, which is characterized in that the element of detection includes
20 kinds of elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo, W, including following step
It is rapid:
(1) sample treatment
S1. after sufentanil citrate being dissolved in water, pH is adjusted with 1% citric acid soln, 2L is settled to ultrapure water, obtains sample
Product mother liquor；
S2. it takes 500 μ L of sample mother liquor in 50mL volumetric flask, is diluted to scale with diluent to get sample solution；
(2) standard solution is prepared；
(3) inner mark solution is prepared；
(4) ICP-MS is tested: sample solution, standard solution, inner mark solution being tested by ICP-MS, obtain each element
Content.
2. analysis method as described in claim 1, which is characterized in that adjust pH with 1% citric acid soln in the step S1
It is 3.7~4.2.
3. analysis method as claimed in claim 2, which is characterized in that adjust pH with 1% citric acid soln in the step S1
It is 3.8.
4. analysis method as described in claim 1, which is characterized in that in the step S2 diluent be concentrated nitric acid, hydrochloric acid and
The mixed solution of 0.1% paregal O -10.
5. analysis method as claimed in claim 4, which is characterized in that the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10
Volume ratio are as follows: (6~10): (0.5~2): 1.
6. analysis method as claimed in claim 5, which is characterized in that the concentrated nitric acid, hydrochloric acid and 0.1% paregal O -10
Volume ratio are as follows: 8:2:1.
7. analysis method as described in claim 1, which is characterized in that the internal standard element of inner mark solution is in the step (3)
Sc, Y and Bi.
8. analysis method as claimed in claim 7, which is characterized in that in the inner mark solution, the concentration of Sc, Y and Bi are each
From for 50~150 μ g/L.
9. analysis method as described in claim 1, which is characterized in that ICP-MS determination condition in the step (4): height takes place frequently
Raw device output power is 1400~1600W；Plasma gas flow velocity is 15~20L/min；Secondary air speed is 1.0~1.4L/
min；Atomization gas flow velocity is 0.85L/min.
10. analysis method as described in claim 1, which is characterized in that the plasma gas and auxiliary gas are respectively argon
Gas and/or helium.
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