CN109632934B - Method for analyzing compatibility of sufentanil citrate and production system - Google Patents
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Abstract
The invention relates to the field of technical analysis of elements in medicines, in particular to an analysis method for compatibility of sufentanil citrate and a production system. The invention relates to an analysis method for the compatibility of sufentanil citrate and a production system, wherein detected elements comprise 20 elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W, and the method comprises the following steps: (1) sample treatment: s1, dissolving sufentanil citrate in water, adjusting the pH value with 1% citric acid solution, and performing constant volume to 2L with ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale with a diluent to obtain a sample solution. (2) Preparing a standard solution; (3) preparing an internal standard solution; (4) ICP-MS test: and testing the sample solution, the standard solution and the internal standard solution by ICP-MS to obtain the content of each element.
Description
Technical Field
The invention relates to the field of technical analysis of elements in medicines, in particular to an analysis method for compatibility of sufentanil citrate and a production system.
Background
Sufentanil, the clinically used citrate, sufentanil citrate, its chemical name is propanamide, N- [4- (methoxymethyl) -1- [2- (2-thienyl) ethyl]-4-piperidinyl]-N-phenyl-2-hydroxy-1,2, 3-propandimethyloate with molecular formula C22H30N2O2S·C6H8O7. Molecular weight 578.66. It was first marketed in the Netherlands in 1983 and it was characterized as white crystals or crystalline powder. Is easily soluble in water and ethanol, and insoluble in chloroform and diethyl ether. Sufentanil citrate is used as an analgesic. Can be used as analgesic during maintenance period of balanced anesthesia. Can be used as anesthetic during induction and maintenance of anesthesia.
The national food and drug administration [2011]430 document issues a notice about the revision of drug standards in the central subsidy place in 2011 and provides requirements for the improvement of 957 drug standards, wherein the notice comprises sufentanil citrate injection.
The key point of the work of improving the quality standard of the fentanyl citrate injection is to improve the quality standard of fentanyl citrate process liquid. Researches find that the control of element content in the sufentanil citrate process liquid is particularly critical to improve the quality standard of the sufentanil citrate process liquid.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides an analysis method for the compatibility of sufentanil citrate and a production system, the detected elements comprise 20 elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W, and the method comprises the following steps:
(1) sample processing
S1, dissolving sufentanil citrate in water, adjusting the pH value with 1% citric acid solution, and performing constant volume to 2L with ultrapure water to obtain a sample mother solution;
s2, sampling 500 mu L of mother liquor of a sample in a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale with a diluent to obtain a sample solution;
(2) preparing a standard solution;
(3) preparing an internal standard solution;
(4) ICP-MS test: and testing the sample solution, the standard solution and the internal standard solution by ICP-MS to obtain the content of each element.
As a preferable technical scheme, the pH value is adjusted to 3.7-4.2 by using 1% citric acid solution in the step S1.
As a preferable technical scheme, the pH is adjusted to 3.8 by using a 1% citric acid solution in the step S1.
As a preferable technical scheme, the diluent in the step S2 is a mixed solution of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10.
As a preferred technical scheme, the volume ratio of the concentrated nitric acid to the hydrochloric acid to the 0.1 percent peregal O-10 is as follows: (6-10): (0.5-2): 1.
as a preferred technical scheme, the volume ratio of the concentrated nitric acid to the hydrochloric acid to the 0.1 percent peregal O-10 is as follows: 8:2: 1.
as a preferred technical solution, the internal standard elements of the internal standard solution in the step (3) are Sc, Y and Bi.
As a preferable technical scheme, the concentrations of Sc, Y and Bi in the internal standard solution are respectively 50-150 mu g/L.
As a preferable technical scheme, in the step (4), the ICP-MS measurement conditions are as follows: the output power of the high-frequency generator is 1400-1600W; the flow rate of the plasma gas is 15-20L/min; the auxiliary airflow speed is 1.0-1.4L/min; the atomization gas flow rate was 0.85L/min.
In a preferred embodiment, the plasma gas and the auxiliary gas are argon and/or helium respectively.
Has the advantages that: the method has good accuracy, and can be used as a test method for measuring 20 elements in sufentanil citrate process liquid. The results show that: the analysis method has good target element linearity, and the detection limit, the accuracy and the like meet the measurement requirements; meanwhile, the method has the advantages of simplicity and convenience in operation, short analysis time, stability, accuracy and the like.
Detailed Description
For purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the problems, the invention provides an analysis method for the compatibility of sufentanil citrate and a production system, detected elements comprise 20 elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W, and the method comprises the following steps:
(1) sample processing
S1, dissolving sufentanil citrate in water, adjusting the pH value with 1 wt% citric acid solution, and fixing the volume to 2L with ultrapure water to obtain a sample mother solution;
s2, sampling 500 mu L of mother liquor, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale with a diluent to obtain a sample solution.
(2) Standard solution preparation
(3) Preparation of internal standard solution
(4) ICP-MS test: and testing the sample solution, the standard solution and the internal standard solution by ICP-MS to obtain the content of each element.
Wherein: preparation of 1% citric acid solution: weighing 200mg of citric acid, and diluting to 20ml with ultrapure water to obtain the final product.
Sample processing
As a preferable technical scheme, the mass of the sufentanil citrate in the step S1 is 75-300 mg.
Preferably, the mass of the sufentanil citrate in the step S1 is 150 mg.
In a preferred embodiment, the pH of the solution is adjusted to 3.7 to 4.2 by using a 1% citric acid solution in step S1.
The inventor conjectures the possible reason that the sufentanil citrate is dissolved by using citric acid, so that foreign impurities cannot be introduced, the matrix effect is weakened, the solubility of the medicine is better by using 1% citric acid solution, and by adjusting the PH to be 3.7-4.2, the medicine can be fully dissolved under the condition and is not easy to decompose or oxidize and deteriorate, the contamination of elements to be detected can be avoided, and the test accuracy is improved; secondly, the density of carbon and carbon-containing polyatomic ions in the plasma can be improved due to the existence of citric acid, and the elements with higher ionization potential can transfer electrons to the carbon and the carbon-containing polyatomic ions, so that the ionization degree of partial elements with higher ionization energy in the plasma is improved.
As a preferred embodiment, the pH of the solution is adjusted to 3.8 with 1% citric acid solution in step S1.
In a preferred embodiment, the diluent in step S2 is a mixed solution of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10.
In a preferred embodiment, the volume ratio of the concentrated nitric acid, the hydrochloric acid and the 0.1% peregal O-10 is: (6-10): (0.5-2): 1.
in a preferred embodiment, the volume ratio of the concentrated nitric acid, the hydrochloric acid and the 0.1% peregal O-10 is: 8:2: 1.
wherein the concentrated nitric acid refers to nitric acid with mass fraction of 68%.
The peregal O-10 refers to fatty alcohol-polyoxyethylene ether, and the peregal O-10 is purchased from Haian petrochemical engineering in Jiangsu province.
Preparing the 0.1% peregal O-10: and taking 100mg of peregal O-10, and using ultrapure water to fix the volume to 100mL to obtain the product.
In the process of research, the inventor finds that nitric acid can prevent small metal oxide particles from being generated, so that metals are in a free state in a solution, but citric acid generates certain resistance to the nitric acid, so that the single metal is incompletely dissolved by using the nitric acid, and individual metal elements are easy to form precipitates in a diluent, so that the dissolution effect of a sample is further improved by compounding hydrochloric acid and nitric acid, but because the hydrochloric acid causes multi-ion atom interference, a certain amount of 0.1% peregal O-10 is added into the diluent for dissolution, and when the volume ratio of the concentrated nitric acid, the hydrochloric acid and the 0.1% peregal O-10 is 8:2:1, the interaction between the diluent and the citric acid can effectively change the intermolecular interaction, the aerosol particle size and the like, so that the transmission rate of an analyte into plasma is increased, the atomization efficiency is improved, the analysis performance is improved, the interference of the analyte to a substrate is minimized, the detection line is lower, and the measurement result is more accurate.
Standard solution preparation
As a preferred embodiment, the standard solution is prepared by the following steps:
absorbing a proper amount of element standard mother liquor, and diluting with a diluent respectively, wherein the prepared standard solution comprises the following components in percentage by weight:
the concentrations of each element of V, Co, Ni, As, Cd, Sb and Pb are respectively 0.1, 0.5, 1,2 and 5 mu g/L.
The Hg element concentration is 0.1, 0.5, 1, 1.5, 2 mug/L.
The concentrations of each element of Li, B, Al, Cr, Mn, Cu and Ba are respectively 10, 20, 50, 100 and 200 mu g/L.
The concentrations of Si, Fe and Zn are respectively 100, 200, 500, 1000 and 2000 mug/L.
Wherein, the specific components and the weight parts of the diluent of the standard solution are synchronous with the step S2.
Preferably, the preparation of the standard solution is specifically performed by:
(1) adding Hg element standard mother liquor 50 μ L, 7 element mixed standard mother liquor 50 μ L, 3 element mixed standard mother liquor 50 μ L, 15 element mixed standard mother liquor 50 μ L, diluting with diluent to scale, and shaking. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 0.1 mu g/L, the concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 10 mu g/L, and the concentrations of Fe, Zn and Si elements are all 100 mu g/L.
(2) Adding Hg element standard mother liquor 250 μ L, 7 element mixed standard mother liquor 250 μ L, 3 element mixed standard mother liquor 250 μ L, 15 element mixed standard mother liquor 100 μ L, diluting with diluent to scale, and shaking. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 0.5 mu g/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 20 mu g/L, and the additive concentrations of Fe, Zn and Si elements are all 200 mu g/L.
(3) Adding Hg element standard mother liquor 500 μ L, 7 element mixed standard mother liquor 500 μ L, 3 element mixed standard mother liquor 500 μ L, 15 element mixed standard mother liquor 250 μ L, diluting with diluent to scale, and shaking. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 1 mug/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 50 mug/L, and the additive concentrations of Fe, Zn and Si elements are all 500 mug/L.
(4) Adding 750 mu L of Hg element standard mother liquor, 1000 mu L of 7 element mixed standard mother liquor, 1000 mu L of 3 element mixed standard mother liquor and 500 mu L of 15 element mixed standard mother liquor, diluting to scale with diluent, and shaking up to obtain the final product. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Mo and W elements are all 2 mug/L, the concentration of Hg element is 1.5 mug/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 100 mug/L, and the additive concentrations of Fe, Zn and Si elements are all 1000 mug/L.
(5) Adding Hg element standard mother liquor 1000 μ L, 7 element mixed standard mother liquor 2500 μ L, 3 element mixed standard mother liquor 2500 μ L, 15 element mixed standard mother liquor 1000 μ L, diluting with diluent to scale, and shaking. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Mo and W elements are all 5 mug/L, the concentration of Hg element is 2 mug/L, the additive standard concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 200 mug/L, and the additive standard concentrations of Fe, Zn and Si elements are all 2000 mug/L.
Specific information of the Hg element standard mother liquor, the 7 element mixed standard mother liquor, the 3 element mixed standard mother liquor and the 15 element mixed standard mother liquor is shown in Table 1.
TABLE 1
Preparation of internal standard solution
As a preferred embodiment, the internal standard elements of the internal standard solution in the step (3) are Sc, Y and Bi.
As a preferred embodiment, the preparation of the internal standard solution comprises the following specific operation steps:
absorbing a proper amount of Sc, Y and Bi element internal standard stock solution with the concentration of 1000mg/L, and diluting the internal standard stock solution to a certain concentration by using a diluent.
In a preferred embodiment, the concentration of Sc, Y and Bi in the internal standard solution is 80-120 μ g/L.
Preferably, the concentrations of Sc, Y and Bi in the internal standard solution are all 100. mu.g/L.
The inventor tests 20 elements (As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W) in a sample, and finds that the test result is more accurate by selecting three elements of Sc, Y and Bi As internal standards, and the inventor conjectures that the sample to be tested does not contain the three elements, and the mass numbers and the first ionization of the three elements are close to the element to be tested, so that the matrix effect is reduced; in addition, the response value of the internal standard element is easily influenced by the matrix, the change of the content of citric acid in the matrix can cause large fluctuation of the internal standard, the matrix sample is properly acidified and diluted, the content of citric acid and the proper internal standard are adjusted, the matrix effect and the acid inhibition effect can be effectively reduced, and the stability and the accuracy of the test result are ensured.
The specific components and the weight parts of the diluent of the internal standard solution are synchronous to the step S2.
ICP-MS testing
As a preferred embodiment, the ICP-MS measurement conditions in the step (4) are: the output power of the high-frequency generator is 1400-1600W; the flow rate of the plasma gas is 15-20L/min; the auxiliary airflow speed is 1.0-1.4L/min; the atomization gas flow rate was 0.85L/min.
Preferably, the ICP-MS determination conditions in the step (4) are as follows: the output power of the high-frequency generator is 1500W; the flow rate of plasma gas is 16L/min; the auxiliary airflow rate is 1.1L/min; the atomization gas flow rate was 0.85L/min.
In a preferred embodiment, the plasma gas and the auxiliary gas are each argon and/or helium.
Preferably, the plasma gas and the auxiliary gas are each argon gas.
As a preferred embodiment, the internal standard elements Sc, Y, Bi are introduced online through a T-shaped injection valve.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
An analysis method for the compatibility of sufentanil citrate and a production system, which detects 20 elements including As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W, comprises the following steps:
(1) sample processing
S1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.7 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution;
s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with a volume ratio of 6:0.5:1 of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 to obtain a sample solution.
(2) Standard solution preparation
The preparation of the standard solution comprises the following specific operations:
(1) and adding 50 mu L of Hg element standard mother liquor, 50 mu L of 7 element mixed standard mother liquor, 50 mu L of 3 element mixed standard mother liquor and 50 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the volumetric flask to a scale by using a diluent, and shaking up the volumetric flask uniformly to obtain the Hg-based catalyst. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 0.1 mu g/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 10 mu g/L, and the additive concentrations of Fe, Zn and Si elements are all 100 mu g/L.
(2) And adding 250 mu L of Hg element standard mother liquor, 250 mu L of 7 element mixed standard mother liquor, 250 mu L of 3 element mixed standard mother liquor and 100 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the volumetric flask to a scale by using a diluent, and shaking up the volumetric flask uniformly to obtain the Hg-based catalyst. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 0.5 mu g/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 20 mu g/L, and the additive concentrations of Fe, Zn and Si elements are all 200 mu g/L.
(3) And (3) adding 500 mu L of Hg element standard mother liquor, 500 mu L of 7 element mixed standard mother liquor, 500 mu L of 3 element mixed standard mother liquor and 250 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the volumetric flask to a scale with a diluent, and shaking up the volumetric flask uniformly to obtain the Hg-doped ZnO semiconductor material. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements are all 1 mug/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 50 mug/L, and the additive concentrations of Fe, Zn and Si elements are all 500 mug/L.
(4) Taking a 50mL volumetric flask, adding 750 muL of Hg element standard mother liquor, 1000 muL of 7 element mixed standard mother liquor, 1000 muL of 3 element mixed standard mother liquor and 500 muL of 15 element mixed standard mother liquor, diluting to a scale with a diluent, and shaking uniformly to obtain the product. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Mo and W elements are all 2 mug/L, the concentration of Hg element is 1.5 mug/L, the additive concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 100 mug/L, and the additive concentrations of Fe, Zn and Si elements are all 1000 mug/L.
(5) And adding 1000 mu L of Hg element standard mother liquor, 2500 mu L of 7 element mixed standard mother liquor, 2500 mu L of 3 element mixed standard mother liquor and 1000 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the volumetric flask to a scale by using a diluent, and shaking the volumetric flask uniformly to obtain the Hg-based composite material. Wherein the concentrations of As, Cd, Co, Ni, Pb, Sb, V, Mo and W elements are all 5 mug/L, the concentration of Hg element is 2 mug/L, the additive standard concentrations of Al, B, Ba, Cr, Cu, Li and Mn elements are all 200 mug/L, and the additive standard concentrations of Fe, Zn and Si elements are all 2000 mug/L.
Wherein, the specific components and the weight parts of the diluent of the standard solution are synchronous with the step S2.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
(3) Preparation of internal standard solution
The preparation of the internal standard solution comprises the following specific operations:
and (3) sucking a proper amount of Sc, Y and Bi element internal standard stock solutions with the concentrations of 1000mg/L, and diluting the internal standard stock solutions to a certain concentration by using a diluent to obtain the high-purity Sc, Y and Bi element internal standard stock solutions.
Wherein, the concentrations of Sc, Y and Bi in the internal standard solution are all 100 mug/L.
The specific components and the weight parts of the diluent of the internal standard solution are synchronous to the step S2.
(4) ICP-MS test: and testing the sample solution, the standard solution and the internal standard solution by ICP-MS to obtain the content of each element.
Wherein, ICP-MS determination conditions are as follows: the output power of the high-frequency generator is 1500W; the flow rate of plasma gas is 16L/min; the auxiliary airflow rate is 1.1L/min; the atomization gas flow rate was 0.85L/min.
The plasma gas and the auxiliary gas are respectively argon gas.
Example 2
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 1, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 4.2 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with a volume ratio of 6:0.5:1 of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 to obtain a sample solution.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
Example 3
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 1, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with a volume ratio of 6:0.5:1 of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 to obtain a sample solution.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
Example 4
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 3, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale by using concentrated nitric acid, hydrochloric acid and a diluent with the volume ratio of 0.1 percent peregal O-10 being 6:2:1 to obtain a sample solution.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
Example 5
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 3, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale by using concentrated nitric acid, hydrochloric acid and a diluent with the volume ratio of 0.1% peregal O-10 of 10:2:1 to obtain a sample solution.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
Example 6
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 3, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale by using concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 diluent with the volume ratio of 8:2:1 to obtain a sample solution.
And (3) carrying out sample injection analysis on the standard solution, and automatically calculating a regression equation by using an instrument by taking the concentration as a horizontal coordinate and the peak area as a vertical coordinate to obtain a linear correlation coefficient R larger than 0.999.
Comparative example 1
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 6, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 2.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale by using concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 diluent with the volume ratio of 8:2:1 to obtain a sample solution.
Comparative example 2
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 6, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 5.0 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor into a 50mL volumetric flask, and diluting the mother liquor to a scale by using concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10 diluent with the volume ratio of 8:2:1 to obtain a sample solution.
Comparative example 3
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 6, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with the volume ratio of concentrated nitric acid to hydrochloric acid being 8:3 to obtain a sample solution.
Comparative example 4
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 7, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with a volume ratio of 8:3 of concentrated nitric acid and 0.1% peregal O-10 to obtain a sample solution.
Comparative example 5
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 7, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with the volume ratio of 8:2:1 of concentrated nitric acid, hydrochloric acid and peregal O-15 to obtain a sample solution.
The Pingtangjia O-15 is purchased from Haian petrochemical engineering in Jiangsu province.
Comparative example 6
The specific steps of an analysis method for the compatibility of sufentanil citrate and a production system are the same as those in example 7, and the differences are that: the sample treatment method comprises the following steps: s1, dissolving 150mg of sufentanil citrate in water, adjusting the pH to 3.8 by using a 1% citric acid solution, and performing constant volume to 2L by using ultrapure water to obtain a sample mother solution; s2, sampling 500 mu L of mother liquor of a sample, putting the mother liquor of the sample into a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale by using a diluent with the volume ratio of 8:2:1 of concentrated nitric acid, hydrochloric acid and peregal O-8 to obtain a sample solution.
The Pingtangjia O-8 is purchased from Haian petrochemical engineering in Jiangsu province.
Performance evaluation
The accuracy, specificity, precision-repeatability of the test methods of the examples and comparative examples were determined. The experimental results of example 6 are shown in table 2, and RSD in the accuracy test is the result measured by three sets of data, and only one set of recovery rate is shown in the table.
(1) And (3) accuracy detection:
preparing low-concentration level solution, medium-concentration level solution and high-concentration level solution, carrying out sample injection analysis, and calculating the recovery rate and the relative standard deviation RSD of the recovery rate in unit percent.
Low concentration level: and (3) sampling 500 mu L of mother liquor of a sample, putting 50 mu L of Hg element standard mother liquor, 50 mu L of 7 element mixed standard mother liquor, 50 mu L of 3 element mixed standard mother liquor and 50 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting to a scale with a diluent, and shaking uniformly to obtain the product. Wherein the element concentration of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W is 0.1 mug/L, the element concentration of Al, B, Ba, Cr, Cu, Li and Mn is 10 mug/L, and the element concentration of Fe, Zn and Si is 100 mug/L. 3 parts of solution are prepared in parallel in the same way.
The medium concentration level: and (3) sampling 500 mu L of mother liquor of a sample, putting the 500 mu L of Hg element mixed standard mother liquor, 500 mu L of 7 element mixed standard mother liquor, 500 mu L of 3 element mixed standard mother liquor and 250 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the mixture to a scale with a diluent, and shaking up to obtain the product. Wherein the concentration of As, Cd, Co, Ni, Pb, Sb, V, Hg, Mo and W elements is 1 mug/L, the concentration of Al, B, Ba, Cr, Cu, Li and Mn elements is 50 mug/L, and the concentration of Fe, Zn and Si elements is 500 mug/L. 3 parts of solution are prepared in parallel in the same way.
High concentration level: and taking 500 mu L of sample mother liquor, putting 750 mu L of Hg element mixed standard mother liquor, 1000 mu L of 7 element mixed standard mother liquor, 1000 mu L of 3 element mixed standard mother liquor and 500 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting to a scale with a diluent, and shaking uniformly to obtain the product. Wherein the concentration of As, Cd, Co, Ni, Pb, Sb and V elements is 2 mug/L, the concentration of Hg element is 1.5 mug/L, the concentration of Al, B, Ba, Cr, Cu, Li and Mn elements is 100 mug/L, and the concentration of Fe, Zn and Si elements is 1000 mug/L. 3 parts of solution are prepared in parallel in the same way.
(2) Detecting specificity: and (3) respectively sampling and analyzing the blank solution, the sample solution and the accuracy solution of the medium concentration level in the process, and calculating the RSD in unit percent.
Preparing a blank solution in the process: putting 500 mu L of water into a 50mL volumetric flask, diluting the water to the scale with a diluent, and shaking up the water to obtain the product.
(3) Precision-repeatability detection: and preparing a repetitive solution for sample injection analysis, and calculating the RSD in unit percent.
Preparing a repetitive solution: and (3) sampling 500 mu L of mother liquor of a sample, putting the 500 mu L of Hg element mixed standard mother liquor, 500 mu L of 7 element mixed standard mother liquor, 500 mu L of 3 element mixed standard mother liquor and 250 mu L of 15 element mixed standard mother liquor into a 50mL volumetric flask, diluting the mixture to a scale with a diluent, and shaking up to obtain the product. Wherein the standard concentration of As, Cd, Co, Ni, Sb, Pb, V, Hg, Mo and W elements is 1 mug/L, the standard concentration of Al, B, Ba, Cr, Cu, Li and Mn elements is 50 mug/L, and the standard concentration of Fe, Zn and Si elements is 500 mug/L. 6 parts of solution are prepared in parallel in the same way.
The diluent for the solution was the same as in each example.
Table 2 example 6 test results
The accuracy (low concentration level), specificity, precision-repeatability of the detection methods of examples 1-5 and comparative examples 1-6 were determined. The data of the V elements are shown in table 3.
TABLE 3V elemental test results
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (3)
1. An analysis method for the compatibility of sufentanil citrate and a production system is characterized in that detected elements comprise 20 elements of As, Cd, B, Al, Si, Cr, Mn, Fe, Zn, Ba, Co, Cu, Hg, Li, Ni, Pb, Sb, V, Mo and W, and the method comprises the following steps:
(1) sample processing
S1, dissolving sufentanil citrate in water, adjusting the pH value with 1% citric acid solution, and performing constant volume to 2L with ultrapure water to obtain a sample mother solution;
s2, sampling 500 mu L of mother liquor of a sample in a 50mL volumetric flask, and diluting the mother liquor of the sample to a scale with a diluent to obtain a sample solution;
(2) preparing a standard solution;
(3) preparing an internal standard solution;
(4) ICP-MS test: the content of each element is obtained by testing the sample solution, the standard solution and the internal standard solution through ICP-MS, the pH value is adjusted to 3.8 by using 1% citric acid solution in the step S1, the diluent in the step S2 is a mixed solution of concentrated nitric acid, hydrochloric acid and 0.1% peregal O-10, and the volume ratio of the concentrated nitric acid to the hydrochloric acid to the 0.1% peregal O-10 is as follows: 8:2:1, the internal standard elements in the step (3) are Sc, Y and Bi, and the concentrations of Sc, Y and Bi in the internal standard solution are all 100 mu g/L.
2. The analytical method according to claim 1, wherein the ICP-MS measurement conditions in the step (4) are: the output power of the high-frequency generator is 1400-1600W; the flow rate of the plasma gas is 15-20L/min; the auxiliary airflow speed is 1.0-1.4L/min; the atomization gas flow rate was 0.85L/min.
3. The analytical method of claim 2, wherein the plasma gas and the auxiliary gas are each argon and/or helium.
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