CN102590180A - Method for detecting element of Chinese medicine, Chinese medicinal extract, soil or medicinal composition containing Chinese medicinal extract - Google Patents
Method for detecting element of Chinese medicine, Chinese medicinal extract, soil or medicinal composition containing Chinese medicinal extract Download PDFInfo
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for determining an element of a Chinese medicine, a Chinese medicinal extract, soil or a medicinal composition containing the Chinese medicinal extract. By the method, a large amount of samples are determined by a seal and heat preservation primary digestion step and an ultrapure water heat preservation dissolution and volume metering step, so that the effects of complete digestion, accurate detection and high repeatability can be achieved.
Description
Technical field
The invention belongs to the analyzing and testing field of medicine, be specifically related to a kind of Chinese crude drug, Chinese medical extract, soil and contain the check and analysis method of constituent content and drug action in the pharmaceutical composition of Chinese medical extract.
Background technology
The Chinese medicine Java brucea is a Simarubaceae brucea plant Java brucea
Brucea javanica(L.) dry mature fruit of Merr.Gather during fruit maturation autumn, removes impurity, dries.The Java brucea beginning is stated from the supplementary Amplifications of the Compendium of Materia Medica that Qing Dynasty's Zhao Xuemin is shown.The effect of recording in the Pharmacopoeia of People's Republic of China is clearing heat and detoxicating, and preventing malaria ends dysentery, the corrosion wart.Be used for dysentery, malaria; Control wart outward, corn.Contain water-soluble components and vegetable oil two parts in the organic principle of Java brucea, its toxic component is present in the water-soluble bitter principle; And the oil-soluble composition, promptly brucea fruit oil avirulence and result of treatment are better, be widely used at present clinical in, the brucea fruit oil extract is used for pharmaceutical formulations, the preparation of commonplace use is Java brucea fruit oil emulsion injection and brucea fruit oil oral latex emulsion.
Many about organic assay and method of quality control in Java brucea medicinal material, extract, the preparation; Range of control also relatively comprehensively, but fewer about the research of the mensuration of constituent content in Java brucea medicinal material, brucea fruit oil and the pharmaceutical composition thereof and method of quality control.For example; Sun Weimin etc. analyze constituent content in 14 kinds of antitumor Chinese medicines; Comprising having analyzed the element in the Java brucea with inductivity coupled plasma mass spectrometry (ICP-MS) method, but only assay determination goes out to comprise totally 26 kinds of elements such as Be, Na, Mg, Al, K, Ca, V.Employing ICP-AES (ICP-AES) methods such as Zhang Xiaolin are measured a large amount of and micro-in 26 kinds of southern medicines comprising Java brucea, but have only measured the K in the Java brucea, Cr, Zn, Cu, Mn and Fe element.Soup is learnt military affairs etc. in trace element and health research; Adopt ICP-AES, atomic fluorescence spectrometry (AFS), flame atomic absorption spectrometry (FAAS) etc. to analyze rare earth or the non-rare earth that comprises the Java brucea medicinal material, element detects detail content such as data in concrete sample preparation step, instrument condition, the Java brucea but do not disclose.Employing flame atomic absorption spectrometrys (FAAS) such as Han Jin soil are measured 11 kinds of trace elements in the 20 kinds of Chinese herbal medicines that comprise Java brucea totally, have only measured the content of the element such as Cu, Mg, Mn of Java brucea.
But it is at present known in 92 kinds of natural elements that occurring in nature exists; Except that inert gas elements (helium, neon, argon, krypton, xenon, radon) and technetium, francium, actinium, protactinium, astatine etc.; Other 81 kinds all are present in the biosome, and wherein certified indispensable element comprises trace elements such as 11 kinds of macroelements and iron, iodine, zinc, selenium, fluorine, copper, cobalt, manganese, chromium, vanadium, nickel, tin, strontium, silicon, bromine, arsenic, boron.Receive the restriction of sample treatment and testing conditions at present, usually the sampling amount of sample is smaller when carrying out element determination, and this causes the detected value of sample in the mensuration process very low, some compositions be difficult to detect or error at measurment very big.But when improving the sampling amount of sample, sample gelatinization occurs, clears up problems such as inhomogeneous or insufficient through regular meeting in digestion process, cause measuring be difficult to carry out or error very big.Particularly to Java brucea or its extract or pharmaceutical composition; At present prior art has generally only been measured Java brucea medicinal material or its extract and has been contained the content of part element in the pharmaceutical composition of extract; Lack simultaneously the content limit of element is studied, more lack Java brucea soil for growth, Chinese crude drug, extract and the relevance that contains the pharmaceutical composition constituent content of extract are studied accordingly.
And the present known digestion procedure of sample, as Microwave Digestion, ashing clear up, acid is cleared up etc., wherein low, the low precision of efficient is cleared up in ashing, usually causes element to be measured (like Pb, Hg, As) volatilization.Though micro-wave digestion is convenient, cost is too high, sample size is little, have potential safety hazard, and it is little to measure elemental range.Most widely used is that acid is cleared up, but traditional acid to clear up maximum problem be to clear up not exclusively, the residual excessive acid of digestion solution can influence the mensuration result, in addition, lacks the unified digestion procedure for vegetable oil, emulsion in the prior art.Therefore; Need therefrom set up the element detection method that a cover is applicable to Chinese crude drug, Chinese medical extract, soil and contains the pharmaceutical composition of Chinese medical extract; It not only can improve the content limit of detection elements; And can adapt to medicinal material, extract and contain the kit detection method of the different associated sample such as pharmaceutical composition constituent content of extract; Especially need set up the digestion procedure that is fit to Java brucea soil for growth, Java brucea medicinal material, brucea fruit oil and 'Brucea fruit oil ' (bruceolic oil emulsion) simultaneously, to increase substantially the element detection level of these samples.
Summary of the invention
The present invention is intended to through Chinese crude drug, Chinese medical extract, soil or the element detection method that contains the pharmaceutical composition of Chinese medical extract are carried out design optimization; The condition of condition that the digestion procedure major control after the optimization is cleared up and final dilution constant volume; Repeatedly clear up processing through what these controls can realize sample; And can be implemented in the very wide sample weighting amount scope and all can clear up, and realized clearing up fully evenly, not gelatinization, reached detect accurately, the element determination effect of favorable reproducibility.Sample solution so that this digestion procedure obtains can be through the content of Instrument measuring element.This method that provides can be applied to medicinal material soil for growth, Chinese crude drug, Chinese medical extract simultaneously and contain the Specimen eliminating of the pharmaceutical composition of Chinese medical extract.
The present invention is specifically through to Java brucea medicinal material, brucea fruit oil, soil or contain the check and analysis of the pharmaceutical composition element of brucea fruit oil; Detect as far as possible comprehensively element; Make the nearly 40 kinds of elements that wherein comprise accurately quantitative simultaneously; Set up one and overlapped all analytical approachs that can survey the content of element and investigate the general characteristic of each element in the pharmaceutical composition that reflects Chinese crude drug, Chinese medical extract and contain extract; And found the relevance of each element in the materials such as medicinal material, the content of each element and the limit form with finger-print is showed.
Particularly; Detection method working sample of the present invention is selected from Chinese crude drug, Chinese medical extract, soil or contains the pharmaceutical composition of Chinese medical extract; Sample can be anticipated before weighing, and processing mode is handled according to the common element method for measuring and got final product, and for example solids such as Chinese crude drug, soil can carry out pulverization process; Contain more a large amount of water in the liquid preparation, be through dewatered process in advance.With the Java brucea is example, and Java brucea medicinal material, soil can carry out pulverization process; Fructus Bruceae extract is that brucea fruit oil can not carry out extra process; Brucea fruit oil emulsion carries out processed.These disposal routes all are relatively known method of this area, and the operation common according to this area gets final product.
Detection method may further comprise the steps:
Claim the appearance step: take by weighing Chinese crude drug, Chinese medical extract, soil or contain the pharmaceutical composition of Chinese medical extract;
The optional step of clearing up in advance: the optional sample that will claim the appearance step adds digestion solution and soaked 2～20 hours;
Clear up step for the first time: the container of clearing up sample for the first time will be housed, and airtight, the baking oven of putting into 130～210 ℃ is incubated 1～24 hour, takes out the back cooling.Container is uncovered, and heating catches up with acid to do to little on 150～210 ℃ of electric hot plates, cooling,
The said sample of clearing up for the first time is:
A) clear up step in advance and soak the acquisition of back adding digestion solution; Or
B) will claim the appearance sample that step obtains, and add digestion solution and obtain;
Dissolving and constant volume step: will be equipped with in the container of the sample after clearing up and add ultrapure water, airtight, put into 100～120 ℃ of baking ovens and be incubated 1～12 hour, take out the back cooling, behind the thin up constant volume, testing sample;
The sample of dissolving and the acquisition of constant volume step is carried out element determination.
In the research of said method, finding in first clearing up closed environment and being controlled under 130～210 ℃ of temperature is key very, this be whole clear up react completely, evenly, a key factor of not gelatinization.In final process for preparation, it also is very crucial putting into 100～120 ℃ of baking ovens insulations at the adding ultrapure water in addition.Satisfying under these two conditions through experiment showed,, the accuracy of mensuration, stability and broad spectrum activity are very good.
In the said method, the about 0.1 ~ 1g of sample sample weighting amount generally speaking, preferably at 0.35 ~ 1g, 0.5g most preferably.
In addition, those skilled in the art can select to carry out the follow-up processing of similarly clearing up as required after clearing up for the first time, and the experiment proof is carried out secondary or cleared up for three times and handle the basic satisfied requirement that detects, and this has further improved the effect of measuring.Certainly after clearing up step three times, those skilled in the art can carry out one or many as required again and clear up.Take all factors into consideration cost and efficiency factor, two to three times are cleared up is proper.
After clearing up for the first time, can comprise further that secondary clears up step in the said method: will clear up the back sample for the first time and add digestion solution, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.After secondary is cleared up step, can further include three times and clear up step: add digestion solution once more in the sample after secondary is cleared up, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.
The present invention is when clearing up step, and preferably heating catches up with acid to do to little on 170～190 ℃ of electric hot plates, more preferably on 180 ℃ of electric hot plates, heats.
In the method for operating of the present invention, clear up step in advance and can carry out as required.For Java brucea medicinal material or brucea fruit oil or contain in the element determination of pharmaceutical composition of brucea fruit oil, when sample is the Java brucea medicinal material, preferably clear up step in advance, more preferably soaked 10 hours; When sample is the soil of brucea fruit oil, Java brucea growth, can not need to clear up in advance.
Further, Java brucea medicinal material of the present invention, brucea fruit oil, soil or the sample determination method that contains the pharmaceutical composition of brucea fruit oil comprise:
Claim an appearance step: take by weighing Java brucea medicinal material, brucea fruit oil, soil or contain the about 0.1 ~ 1g of sample of the pharmaceutical composition of brucea fruit oil, preferred 0.35g ~ 1g, most preferably 0.5g;
The optional step of clearing up in advance: the optional sample that will claim the appearance step adds digestion solution immersion 2～20 hours; Wherein, when sample is the Java brucea medicinal material, preferably soaked 10 hours;
Clear up step for the first time: the container of clearing up sample for the first time will be housed, and airtight, the baking oven of putting into 130～210 ℃ is incubated 1～24 hour, takes out the back cooling, and container is uncovered, and heating catches up with acid to do to little on 150～210 ℃ of electric hot plates, cooling,
The said sample of clearing up for the first time is:
A) clear up step in advance and soak the acquisition of back adding digestion solution; Or
B) will claim the appearance sample that step obtains, and add digestion solution and obtain;
Dissolving and constant volume step: will be equipped with in the container of the sample after clearing up and add ultrapure water, airtight, put into 100～120 ℃ of baking ovens and be incubated 1～12 hour, take out the back cooling, the thin up constant volume, to be measured after shaking up, preferably use the plastic bottle constant volume;
The sample that dissolving constant volume step is obtained carries out element determination.
After clearing up for the first time, can comprise further that secondary clears up step in the said method: will clear up the back sample for the first time and add digestion solution, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.After secondary is cleared up step, also can further comprise and clear up step three times: add digestion solution once more in the sample after secondary is cleared up, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.After clearing up step three times, can carry out one or many again clears up.
The digestion solution that adds in each step in the said method is the general reagent of clearing up in this area; Can be selected from nitric acid, hydrogen peroxide, hydrofluorite, perchloric acid, hydrochloric acid, sulfuric acid, potassium persulfate, potassium hydrogen persulfate, sodium peroxydisulfate, hydrogen persulfate sodium, phosphoric acid, hydrobromic acid, or two or more materials is any than combination.
In the said method, when specifically clearing up step in advance to the Java brucea medicinal material, digestion solution preferably uses the hydrogen peroxide immersion to clear up in advance, preferred 2ml hydrogen peroxide/0.5g Java brucea medicinal material.
In the said method, when clearing up for the first time, brucea fruit oil is cleared up for the first time and can be used nitric acid or hydrogen peroxide, the preferably combination of nitric acid and hydrogen peroxide, and every 0.5g brucea fruit oil uses the effect of 5ml nitric acid and 2ml hydrogen peroxide best; The Java brucea soil for growth is cleared up for the first time and can be used nitric acid or hydrofluorite, the preferably combination of nitric acid and hydrofluorite, and the effect of every 0.5g pedotheque 3ml nitric acid and 5ml hydrofluorite is best; The Java brucea medicinal material is cleared up for the first time can be according to the use of whether clearing up step adjustment digestion solution in advance; For example: as clear up in advance step then digestion solution can directly add digestion solution in the potpourri after clearing up in advance; The preferred nitric acid that uses, every 0.5g Java brucea medicinal material uses the effect of 5ml nitric acid best, then can directly add digestion solution as not clearing up step in advance; The preferably combination of nitric acid and hydrogen peroxide, every 0.5g Java brucea medicinal material use the effect of 5ml nitric acid and 2ml hydrogen peroxide best.
In the said method, step and other follow-up clearing up in the step, the preferred nitric acid of the digestion solution of use are cleared up, cleared up for three times to secondary.Every 0.5g claims that the sample of appearance adds digestion solution 1～10ml, more preferably 1ml digestion solution.
In the said method, the said holding temperature of clearing up baking oven in the step for the first time is 180～200 ℃, preferred 190 ℃; Temperature retention time is 10～14 hours, preferred 12 hours.
In the said method, preferred saidly clear up that to catch up with acid in heating on the electric hot plate in the step be on 170～190 ℃ of electric hot plates, to heat, more preferably on 180 ℃ of electric hot plates, heat.
In the said method, temperature of oven is preferred 105～115 ℃ in said dissolving and the constant volume step, more preferably 110 ℃; Preferred 3～10 hours of temperature retention time, more preferably 4 hours.
Constituent content is measured
According to method of the present invention sample is handled laggard row element and measure, described assay method can carry out according to the method for carrying out element determination in this area usually.
Instrument and the method for measuring constituent content at present mainly contain atomic absorption spectrography (AAS) (AAS), atomic fluorescence spectrometry (AFS), the chromatography of ions (IC), inductively coupled plasma emission spectrography (ICP-AES, ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), neutron activation analysis method (INAA), x ray fluorescence spectrometry (XRF) etc.Measure the determination of trace element appearance of specific sample and element-specific in addition.In above these assay methods; Inductively coupled plasma mass spectrometry have sensitivity the highest, once can measure multiple element, advantage such as easy to use; As most preferred method, other instrument and method or its various combinations are as less preferred or additional method with inductively coupled plasma mass spectrometry in the present invention.
ICP-MS measures preferably measuring by following condition of constituent content: RF power: between 1200w～1600w, and preferred 1300w～1400w, cold gas flow velocity: 16L/min; Secondary air speed: 1.0L/min, atomization gas flow velocity: 0.8L/min, sampling depth: 8mm; Sampling spiroid aperture: 1.0mm; Intercepting taper hole footpath: 0.7mm, sample promotes speed: 0.4ml/min, atomization temperature: 2 ℃.Under these conditions, adopt the ICP-MS method, each element in the sample is carried out assay, every duplicate samples replicate determination 3 times obtains the constituent content result.
Draw the element finger-print
Each constituent content value of measuring is depicted as the element finger-print, and the element finger-print comprises 2 kinds of collection of illustrative plates.
First kind of collection of illustrative plates is the safe level finger-print, draws 2 curves with measuring the element that has the safe level value among the result, safe level curve and mensuration curve.With the element sequence number is horizontal ordinate, is ordinate with the logarithm value of element limit value, and the curve of drafting is the safe level curve.With the element sequence number is horizontal ordinate, and the logarithm value of constituent content is an ordinate, and the curve of drafting is for measuring curve (constituent content is 0ng/g or is meaningless by its logarithm value that measured value is calculated as negative value, counts 0 without exception in this case).The safe level collection of illustrative plates can judge whether each element exceeds safe level in the medicine; Require to measure curve fully under the safe level typical curve; If two have coincide point or point of crossing promptly to judge have element to exceed safe level between the curve, for defective medicine or need be applied to clinical conditionally.
Second kind of collection of illustrative plates is the constituent content finger-print; Element with all mensuration is drawn a curve; With the element sequence number is horizontal ordinate; With the logarithm value of constituent content is ordinate (constituent content is 0ng/g or is meaningless by its logarithm value that measured value is calculated as negative value, counts 0 without exception in this case), draws the constituent content curve.The constituent content finger-print can intuitive judgment and can be according to the content of each element in the medicine, differentiates that the medicinal material true and false is good and bad, distinguishes the effect that the characteristics such as Changing Pattern of Chinese crude drug-extract-preparation are produced in medicinal material and substitute, the discriminating medicinal material place of production, reflection.
Because what chromatographic fingerprints of Chinese materia medica and spectral fingerprint collection of illustrative plates mainly reflected is the characteristic of organic compound in the Chinese medicine; Has the effect of distinguishing the medicinal material place of production and the medicinal material true and false; But because the difference of the weather in each place of production each year (each crop cycle), rainfall amount, humidity, temperature, season alternation, sunshine-duration, wind direction, wind speed etc.; The finger-print of reflection organic compound characteristic is not exclusively fixing; And spectrum and chromatographic fingerprinting all only have semiquantitative characteristics, and this is a limitation of chromatogram and spectral fingerprint collection of illustrative plates.But because each content of elements is in a metastable state in the earth's crust in each place of production of medicinal material; The whole finger-print characteristic of each element mainly receives the influence in the Java brucea medicinal material place of production in the Chinese medicine Java brucea medicinal material; Promptly plant the influence of content of the metal elements in soil of Java brucea medicinal material; Therefore, reflect that the element finger-print of each place of production medicinal material elemental characteristic can belong to the place of production of medicinal material more accurately, and the content of each element is accurately quantitative in the element finger-print; Have the function of independent each constituent content of reflection concurrently, this is the essential thinking of this notion of fingerprint collection of illustrative plates: not only reflected whole macrofeature, but also embodied the microscopic feature of each element.
The element finger-print curve of unknown medicinal material and known each place of production medicinal material, genunie medicinal materials is carried out similarity relatively, can judge medicinal material the place of production, whether be genuine piece, whether be genunie medicinal materials.
Element finger-print difficulty is judged the difference between medicinal material quality product and the poor products; Difference between quality product and the poor products is that mainly the drug effect of medicine is good and bad; And generally be organic analysis with the direct relevant quality control of drug effect, at this moment can combine chromatogram, spectral fingerprint collection of illustrative plates and element finger-print comprehensive evaluation medicinal material.
The characteristics such as Changing Pattern of Chinese crude drug-extract-preparation are produced in reflection
Chinese crude drug obtains in the process of extract and preparation through steps such as extraction, preparations; Each element attenuating or even the disappearance (detect less than) of content can occur, also possibly occur the raising of some constituent contents owing to the reason of technology in the Chinese crude drug, and the Changing Pattern of element finger-print can be used as the means of accurate control stable processing technique homogeneous between research Chinese crude drug-extract-preparation.
The production technology of stable uniform must have stable element finger-print Changing Pattern, and this provides important reference and replenish for traditional production run control of carrying out with reference to quality standard.The element-specific that also can avoid possibly existing in the Chinese medicine production run is polluted.
Advantage of the present invention is:
1, digestion procedure provided by the invention disturbs and lacks, and clears up fully, and accuracy of measurement is high, and it is extensive to be suitable for sample, is applicable to soil, medicinal material, extract and preparation thereof.This method has realized the multielement simultaneous determination of sample, has confirmed that through precision, repeatability, accuracy experimental result this method can accurately measure the content of more than 40 kind of element.
2, of the present invention clear up and final compound method has realized the element of Chinese medical extract and preparation is accurately comprehensively measured; The utilization of this method is for the Changing Pattern of element finger-print between research Chinese crude drug-extract-preparation; Accurately each link of control Chinese medicine production all plays an important role, and is to weigh the whether important detection method of stable uniform of product technology.
3, the present invention accurately shows the potential safety hazard of the element form with finger-print all sidedly, and the safe level of element derives from the standards of pharmacopoeia and the industry standard of various countries, can directly control product quality, has guaranteed clinical drug safety.
The similarity of the element finger-print that 4, obtains through the present invention relatively, judge medicinal material the place of production, whether be genuine piece, whether be that genunie medicinal materials are more accurate.
Description of drawings
The safe level finger-print of Fig. 1 Java brucea medicinal material
The constituent content finger-print of Fig. 2 Java brucea medicinal material
Embodiment
(1) claims appearance: the Java brucea medicinal material fine powder that takes by weighing about 0.5g;
(2) clear up in advance: fine powder is added in the teflon of high-pressure digestion jar in the pipe, adds 2ml hydrogen peroxide (top grade is pure), soaked 10 hours;
(3) clear up for the first time: will be equipped with in the above-mentioned teflon of clearing up sample in advance and directly add 5ml nitric acid (senior pure) again in the pipe; Pipe in the teflon is put into the high-pressure digestion jar; The high-pressure digestion potting is screwed well, and the baking oven of putting into 190 ℃ is incubated 12 hours, takes out the back cooling.Catch up with acid to do cooling to little the heating on 180 ℃ of electric hot plates of pipe in the teflon.
(4) dissolving and constant volume: adding 10ml left and right sides ultrapure water in the interior pipe of the teflon of clearing up the back sample will be housed; Pipe in the teflon is put into the high-pressure digestion jar, the high-pressure digestion potting is screwed well, put into 110 ℃ of baking oven insulations 4 hours; Take out the back cooling, thin up is to 25ml.Change over to after shaking up in the special plastic sample bottle, number to be measured.
Do the retinue contrast with standard substance synchronously, and it is blank to do omnidistance preface, measures with ICP-MS, the result sees the following form:
Table 1 embodiment 1 element determination result
Massfraction: ng/g (10
-9)
Detection is less than Nd
The comparative example 1
Step (1), (2), (4) are with embodiment 1, step (3) as follows:
(3) clear up for the first time: the baking oven of unencapsulated high-pressure digestion jar being put into 190 ℃ is incubated 12 hours, takes out the back cooling.Catch up with acid to do cooling to little the heating on 180 ℃ of electric hot plates of pipe in the teflon.
Experiment sample gelatinization, sample occur and loses in a large number and cross pollution when proceeding to step (3), causes experiment to proceed.
The comparative example 2
Step (1), (2), (4) are with embodiment 1, step (3) as follows:
(3) clear up for the first time: the high-pressure digestion potting is screwed well, and the baking oven of putting into 240 ℃ is incubated 12 hours, takes out the back cooling.Catch up with acid to do cooling to little the heating on 180 ℃ of electric hot plates of pipe in the teflon.
Do the retinue contrast with standard substance synchronously, and it is blank to do omnidistance preface, measures with ICP-MS, the result sees the following form:
Table 2 comparative example 2 element determination results
Massfraction: ng/g (10
-9)
Detection is less than Nd
The comparative example 3
Step (1)～(3) are with embodiment 1, step (4) as follows:
(4) dissolving and constant volume: adding 10ml left and right sides ultrapure water in the interior pipe of the teflon of clearing up the back sample will be housed; Pipe in the teflon is put into the high-pressure digestion jar, the high-pressure digestion potting is screwed well, put into 80 ℃ of baking oven insulations 4 hours; Take out the back cooling, thin up is to 25ml.Change over to after shaking up in the special plastic sample bottle, number to be measured.
Do the retinue contrast with standard substance synchronously, and it is blank to do omnidistance preface, measures with ICP-MS, the result sees the following form:
Table 3 comparative example 3 element determination results
Massfraction: ng/g (10
-9)
Detection is less than Nd
Brief summary: can find out by above-mentioned experiment, the first digestion procedure that the present invention uses, the basic free of losses of element, determination data is more parallel, and (RSD) is little for relative standard deviation, and result precision is high.
Sample dissolution after clearing up and constant volume process make mensuration more stable.
Step (1)～(3) are with embodiment 1, step (4)～(6) as follows:
(4) secondary is cleared up: will be equipped with in the teflon of clearing up the back sample for the first time and add 1ml nitric acid (senior pure) in the pipe, heating catches up with acid to do cooling to little on 180 ℃ of electric hot plates.
Clear up for (5) three times: add 1ml nitric acid (senior pure) in the sample after secondary is cleared up once more, heating catches up with acid to do cooling to little on 180 ℃ of electric hot plates;
(6) dissolving and constant volume: adding 10ml left and right sides ultrapure water in the interior pipe of the teflon of clearing up the back sample will be housed; Pipe in the teflon is put into the high-pressure digestion jar, the high-pressure digestion potting is screwed well, put into 110 ℃ of baking oven insulations 4 hours; Take out the back cooling, thin up is to 25ml.Change over to after shaking up in the special plastic sample bottle, number to be measured.
Do the retinue contrast with standard substance synchronously, and it is blank to do omnidistance preface, measures with ICP-MS, the result sees the following form:
Table 4 embodiment 2 element determination results
Massfraction: ng/g (10
-9)
Detection is less than Nd
Brief summary: owing to contain halogen in the sample; These halogens can form a certain amount of halogen acid in digestion process, find that in the mensuration process halogen acid has certain infringement to experimental apparatus, after clearing up through two or three times; Halogen acid is further removed, and has reduced the infringement to instrument.
In addition; Find also that in experiment though the testing sample that Java brucea is cleared up is for the first time relatively clarified, some other Chinese medicine samples are cleared up the back testing sample for the first time and clarified inadequately or uneven phenomenon arranged; After clearing up through two or three times, sample can reach the clarification effect of uniform.
(1) claims appearance: take by weighing the brucea fruit oil of about 0.5g, be added to the interior pipe of teflon of high-pressure digestion jar
In, add 5ml nitric acid (senior pure), 2ml hydrogen peroxide (top grade is pure);
(2) clear up for the first time: the interior pipe of teflon that above-mentioned sample will be housed is put into the high-pressure digestion jar, and the high-pressure digestion potting is screwed well, and the baking oven of putting into 210 ℃ is incubated 20 hours, takes out the back and cools off; Catch up with acid to do cooling to little the heating on 180 ℃ of electric hot plates of pipe in the teflon.
(3) secondary is cleared up: will be equipped with and add 1ml nitric acid (senior pure) in the teflon of the sample after clearing up for the first time in the pipe, heating catches up with acid to do cooling to little on 180 ℃ of electric hot plates;
Clear up for (4) three times: add 1ml nitric acid (senior pure) in the sample after secondary is cleared up once more, heating catches up with acid to do cooling to little on 180 ℃ of electric hot plates;
(5) dissolving and constant volume: adding 10ml left and right sides ultrapure water in the interior pipe of the teflon of clearing up the back sample will be housed; Pipe in the teflon is put into the high-pressure digestion jar, the high-pressure digestion potting is screwed well, put into 100 ℃ of baking oven insulations 10 hours; Take out the back cooling, thin up is to 25ml.Change over to after shaking up in the special plastic sample bottle, numbering (or mark title) back is to be measured.
Do the retinue contrast with standard substance synchronously, and it is blank to do omnidistance preface, measures with ICP-MS, the result sees the following form:
Table 5 embodiment 3 element determination results
Massfraction: ng/g (10
-9)
Detection is less than Nd
(genseng is one of time-honored rare Chinese medicine, and modern Chinese herbal medicine is learned research and shown that polysaccharide is the effective constituent of genseng, and its pharmacological activity is embodied in many aspects, like antitumor, hypoglycemic, antifatigue, anti-oxidant and immunological regulation etc. to get the panaxan.
The panaxan is to be the effective part extract of principal ingredient with the polysaccharide that from genseng, extracts), carrying out element determination according to the step of embodiment 2, the result is following:
Table 6 embodiment 4 element determination results
Massfraction: ng/g (10
-9)
Detection is less than Nd
Element determination result with Java brucea among the embodiment 2 draws the element finger-print.
The drafting of safe level finger-print: draw 2 curves with measuring the element that has the safe level value among the result, safe level curve and mensuration curve.With the element sequence number is horizontal ordinate, is ordinate with the logarithm value of element limit value, and the curve of drafting is the safe level curve.With the element sequence number is horizontal ordinate, and the logarithm value of constituent content is an ordinate, and the curve of drafting is for measuring curve (constituent content is 0ng/g or is meaningless by its logarithm value that measured value is calculated as negative value, counts 0 without exception in this case).The safe level collection of illustrative plates can judge whether each element exceeds safe level in the medicine; Require to measure curve fully under the safe level typical curve; If two have coincide point or point of crossing promptly to judge have element to exceed safe level between the curve, for defective medicine or need be applied to clinical conditionally.
The drafting of constituent content finger-print: the element with all mensuration is drawn a curve; With the element sequence number is horizontal ordinate; With the logarithm value of constituent content is that (constituent content is 0ng/g or is meaningless by its logarithm value that measured value is calculated as negative value ordinate; Count 0 without exception in this case), draw the constituent content curve.The constituent content finger-print can intuitive judgment and can be according to the content of each element in the medicine, differentiates that the medicinal material true and false is good and bad, distinguishes the effect that the characteristics such as Changing Pattern of Chinese crude drug-extract-preparation are produced in medicinal material and substitute, the discriminating medicinal material place of production, reflection.
Claims (16)
1. the method for a working sample constituent content, said sample is selected from Chinese crude drug, Chinese medical extract, soil or contains the pharmaceutical composition of Chinese medical extract, said method comprising the steps of:
Claim an appearance step: take by weighing Chinese crude drug, Chinese medical extract, soil or contain the pharmaceutical composition of Chinese medical extract;
The optional step of clearing up in advance: the optional sample that will claim the appearance step adds digestion solution immersion 2～20 hours;
Clear up step for the first time: the container of clearing up sample for the first time will be housed, and airtight, the baking oven of putting into 130～210 ℃ is incubated 1～24 hour, takes out the back cooling, and container is uncovered, and heating catches up with acid to do to little on 150～210 ℃ of electric hot plates, cooling,
The said sample of clearing up for the first time is:
A) clear up step in advance and soak the acquisition of back adding digestion solution; Or
B) will claim the appearance sample that step obtains, and add digestion solution and obtain;
Dissolving and constant volume step: will be equipped with in the container of the sample after clearing up and add ultrapure water, airtight, put into 100～120 ℃ of baking ovens and be incubated 1～12 hour, take out the back cooling, behind the thin up constant volume, get testing sample;
The sample of dissolving and the acquisition of constant volume step is carried out element determination.
2. the method for claim 1 is characterized in that, when said working sample is Chinese crude drug, clears up step in advance.
3. according to claim 1 or claim 2 method is characterized in that, said Chinese crude drug, Chinese medical extract or the pharmaceutical composition that contains Chinese medical extract are respectively Java brucea medicinal material or brucea fruit oil or the pharmaceutical composition that contains brucea fruit oil.
4. method as claimed in claim 3 is characterized in that, said method comprising the steps of:
Claim an appearance step: take by weighing Java brucea medicinal material, brucea fruit oil, soil or contain the about 0.1 ~ 1g of sample of the pharmaceutical composition of brucea fruit oil, preferred 0.35g ~ 1g, most preferably 0.5g;
The optional step of clearing up in advance: the optional sample that will claim the appearance step adds digestion solution immersion 2～20 hours; Wherein, when sample is the Java brucea medicinal material, preferably soaked 10 hours;
Clear up step for the first time: the container of clearing up sample for the first time will be housed, and airtight, the baking oven of putting into 130～210 ℃ is incubated 1～24 hour, takes out the back cooling, and container is uncovered, and heating catches up with acid to do to little on 150～210 ℃ of electric hot plates, cooling,
The said sample of clearing up for the first time is:
A) clear up step in advance and soak the acquisition of back adding digestion solution; Or
B) will claim the appearance sample that step obtains, and add digestion solution and obtain;
Dissolving and constant volume step: will be equipped with in the container of the sample after clearing up and add ultrapure water, airtight, put into 100～120 ℃ of baking ovens and be incubated 1～12 hour, take out the back cooling, the thin up constant volume, to be measured after shaking up, preferably use the plastic bottle constant volume;
The sample that dissolving constant volume step is obtained carries out element determination.
5. like any described method of claim 1-4; It is characterized in that said dissolving and constant volume step operate by following mode: add about 10ml ultrapure water; Put into 100～120 ℃ of baking ovens and be incubated 1～12 hour, take out the back cooling, thin up is to 25ml; It is to be measured to shake up the back, preferably uses the plastic bottle constant volume.
6. like any described method of claim 1-4, it is characterized in that the said temperature of clearing up the insulation of step for the first time is 180～200 ℃, preferred 190 ℃.
7. like any described method of claim 1-4, it is characterized in that said to clear up the time that is incubated in the step for the first time be 10 ~ 14 hours, preferred 12 hours.
8. like any described method of claim 1-4, it is characterized in that the temperature that is incubated in said dissolving and the constant volume step is 105～115 ℃, preferred 110 ℃.
9. like any described method of claim 1-4, it is characterized in that the time of said dissolving and the insulation of constant volume step is 3 ~ 10 hours, preferred 4 hours.
10. like any described method of claim 1-9, it is characterized in that said method is carried out secondary and cleared up step after clearing up for the first time: will clear up the back sample for the first time and add digestion solution, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.
11. method as claimed in claim 10 is characterized in that, said method carries out clearing up step three times after secondary is cleared up step: add digestion solution in the sample after secondary is cleared up, heating catches up with acid to do cooling to little on 150～210 ℃ of electric hot plates.
12. method as claimed in claim 11 is characterized in that, said method is carried out one or many again and is cleared up after clearing up step three times.
13. as aforementioned any described method of claim, it is characterized in that, saidly clear up in the step that to catch up with acid in heating on the electric hot plate be on 170～190 ℃ of electric hot plates, to heat, more preferably on 180 ℃ of electric hot plates, heat.
14. method as claimed in claim 4 is characterized in that, clears up step when working sample is the Java brucea medicinal material in advance, the said digestion solution of clearing up step in advance uses the hydrogen peroxide immersion to clear up in advance, preferred 2ml hydrogen peroxide/0.5g Java brucea medicinal material.
15. like the said method of claim 4; When the said sample of clearing up for the first time is brucea fruit oil; Said first digestion solution is nitric acid or hydrogen peroxide, the preferably combination of nitric acid and hydrogen peroxide, and most preferably every 0.5g brucea fruit oil uses 5ml nitric acid and 2ml hydrogen peroxide; During Java brucea medicinal material after said sample is to clear up step in advance, digestion solution is a nitric acid, and preferred every 0.5g Java brucea medicinal material uses 5ml nitric acid.
16., it is characterized in that other after clearing up for the first time like any described method of claim 10-12
When clearing up step, every 0.5g claims that the sample of appearance adds 1 to 10ml digestion solution, more preferably 1ml digestion solution; Preferred said digestion solution is a nitric acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105241741A (en) * | 2015-11-27 | 2016-01-13 | 广西壮族自治区药用植物园 | Pretreatment method for detecting metal elements in kapok powder |
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| CN105241741A (en) * | 2015-11-27 | 2016-01-13 | 广西壮族自治区药用植物园 | Pretreatment method for detecting metal elements in kapok powder |
| CN105241741B (en) * | 2015-11-27 | 2018-03-30 | 广西壮族自治区药用植物园 | Detect the pre-treating method of metallic element in common bombax flower powder |
| CN109632931A (en) * | 2018-12-29 | 2019-04-16 | 上海微谱化工技术服务有限公司 | A kind of analysis method of midazolam formulation |
| CN109632930A (en) * | 2018-12-29 | 2019-04-16 | 上海微谱化工技术服务有限公司 | A kind of analysis method of midazolam and production system compatibility |
| CN109632931B (en) * | 2018-12-29 | 2021-07-30 | 上海微谱化工技术服务有限公司 | Analysis method of midazolam preparation |
| CN109632930B (en) * | 2018-12-29 | 2022-01-25 | 上海微谱化工技术服务有限公司 | Analysis method for compatibility of midazolam and production system |
| CN110412018A (en) * | 2019-09-09 | 2019-11-05 | 华东师范大学 | The detection method of P elements in a kind of plant |
| CN110632162A (en) * | 2019-09-11 | 2019-12-31 | 山西大学 | Method for identifying wild astragalus and cultivated astragalus in ground |
| CN110632162B (en) * | 2019-09-11 | 2021-07-27 | 山西大学 | Method for identifying wild astragalus and cultivated astragalus in ground |
| CN110702773A (en) * | 2019-11-20 | 2020-01-17 | 武汉上谱分析科技有限责任公司 | Method for measuring Pb isotope ratio in sulfide by using MC-ICP-MS |
| CN110702773B (en) * | 2019-11-20 | 2020-11-03 | 武汉上谱分析科技有限责任公司 | Method for measuring Pb isotope ratio in sulfide by using MC-ICP-MS |
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