CN107621510A - A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug - Google Patents
A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug Download PDFInfo
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- CN107621510A CN107621510A CN201710903565.4A CN201710903565A CN107621510A CN 107621510 A CN107621510 A CN 107621510A CN 201710903565 A CN201710903565 A CN 201710903565A CN 107621510 A CN107621510 A CN 107621510A
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- filter residue
- puerarin
- bulk drug
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Abstract
A kind of technique for being used to detect metal impurities in Puerarin bulk drug, comprises the following steps：The first step：The root of kudzu vine is crushed, the screenings obtained after 50~100 mesh sieves excessively, which is immersed in hydrochloric acid solution, to be handled；Second step：The pH value of the system of the first step is adjusted to neutrality, is then filtrated to get filter residue；3rd step：The filter residue obtained with dioxygen water process second step, washs after terminating, filters to take filter residue, the filter residue after then the filter residue is dried；4th step：EDTA solution and sodium hydroxide solution are added to the filter residue after the drying, stirring reaction 1~3 hour under the conditions of 25~35 DEG C；5th step：The supernatant for taking the 4th step to obtain, using the content of high performance liquid chromatography detection wherein metal ion.After the pre-treating technology processing of the present invention, the content of metal ion in the root of kudzu vine can be accurately detected.
Description
Technical field
It is more particularly to a kind of to be used to detect Puerarin bulk drug the present invention relates to a kind of detection method of kish impurity
The pre-treating technology of middle metal impurities, belongs to analytical chemistry field.
Background technology
The general name of the materials such as heavy metal, arsenic and catalyst that the metal impurities in medicine are known as, wherein relating to
And to many transition metals and metalloid element.Initiation material, catalyst, accessory substance in chemical drugs building-up process, not
Metal impurities may be introduced by reacting the metal tools of complete reagent, canister, pipeline and other not acid and alkali-resistances, and former
Metal residue in auxiliary material further can be brought into pharmaceutical preparation.These metal impurities are generally without therapeutic action, based on medicine
The requirement of thing security and quality control should be controlled strictly, and European Medicines Agency promulgated metallic catalyst in 2008
Or policy paper as defined in metal reagent residual quantity limit, and formally implement in the range of European Union.
At present, the metal ion that pharmacopoeia of each country records still carries out semiquantitative determination with heavy metal inspection technique with optical colorimetry
Based on, these classical ways exist specificity is poor, sensitivity is low, operation is loaded down with trivial details, using toxic reagent the shortcomings of, also can not be overall
Investigate the metal impurities in medicine, it is therefore necessary to introduce more advanced, more easily alternative.USP is newly-increased in its plan
Annex<233>Soliciting in original text for metal impurities inspection technique recommends 2 kinds of instrumental methods, i.e. inductively coupled plasma transmitting light
Spectrometry（ICP-AES）And inductively coupled plasma mass spectrometry（ICP- MS）, to substitute existing heavy metal inspection technique.USP
The oxaliplatin bulk drug that 32 enlarged editions record is i.e. using 6 kinds of metals such as ICP-AES methods measure cadmium, chromium, copper, iron, nickel, lead
Impurity, using yttrium as internal standard substance.
ICP-AES methods have that test limit is low, the degree of accuracy is high, dynamic linear response range is wide and multiple element while measure etc. are excellent
Point, there is certain competitiveness in terms of inorganic analysis, be widely used to chemical industry, geology, material, environment and biological sample
Deng numerous areas, but the application in Pharmaceutical Analysis, particularly Chinese medicine has no report.
The content of the invention
It is an object of the invention to provide a kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug.
In order to achieve the above objects and other related objects, technical scheme provided by the invention is：One kind is used to detect the root of kudzu vine
The technique of metal impurities, comprises the following steps in plain bulk drug：
The first step：The root of kudzu vine is crushed, the screenings obtained after 50~100 mesh sieves excessively, which is immersed in hydrochloric acid solution, to be handled；
Second step：The pH value of the system of the first step is adjusted to neutrality, is then filtrated to get filter residue；
3rd step：The filter residue obtained with dioxygen water process second step, washs after terminating, filters to take filter residue, then by the filter residue
Filter residue after being dried；
4th step：EDTA solution and sodium hydroxide solution are added to the filter residue after the drying, is stirred under the conditions of 25~35 DEG C anti-
Answer 1~3 hour；
5th step：The supernatant for taking the 4th step to obtain, using the content of high performance liquid chromatography detection wherein metal ion.
Preferably technical scheme is：In the first step：Screenings is immersed in 0.05~0.1mol/L hydrochloric acid solutions and carried out
Processing 1 ~ 3 hour.
Preferably technical scheme is：In second step：Using 0.05~0.1mol/L sodium hydroxide solution, by the first step
The pH value of system adjust to neutrality.
Preferably technical scheme is：In the third step：Obtained with the dioxygen water process second step that mass fraction is 0.1~0.3%
The filter residue obtained, is washed with deionized 2 ~ 3 times after terminating.
Preferably technical scheme is：In the third step：By the filter residue under the conditions of 55 ~ 65 DEG C, after drying obtains drying
Filter residue.
Because above-mentioned technical proposal is used, the present invention this have the advantage that compared with prior art：
After the pre-treating technology processing of the present invention, the content of metal ion in the root of kudzu vine can be accurately detected.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this implementation
Content disclosed by example understands other advantages and effect of the present invention easily.
Embodiment 1：A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug
（1）The root of kudzu vine is taken, is ground into powder, 50 mesh sieves is crossed, is then immersed in 0.05mol/L hydrochloric acid solution, is handled 1 hour.
（2）To step（1）System in add 0.05mol/L sodium hydroxide solution, regulation pH value is to neutrality, then mistake
Filtrate is filtered out, obtains filter residue.
（3）Use mass fraction for 0.1% dioxygen water treatment steps（2）The filter residue of collection, after washing 2 times, filter to take filter
Slag, then filter residue is placed under the conditions of 55 DEG C and dried.
（4）Take step（3）Filter residue after drying, adds EDTA solution and sodium hydroxide solution thereto, under the conditions of 25 DEG C
Stirring reaction 1 hour.
（5）Take step（4）Reacted supernatant, using the content of high performance liquid chromatography detection wherein metal ion.
Embodiment 2：A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug
A kind of technique for being used to detect metal impurities in Puerarin bulk drug, the technique comprise the following steps：
（1）The root of kudzu vine is taken, is ground into powder, 70 mesh sieves is crossed, is then immersed in 0.08mol/L hydrochloric acid solution, is handled 2 hours.
（2）To step（1）System in add 0.08mol/L sodium hydroxide solution, regulation pH value is to neutrality, then mistake
Filtrate is filtered out, obtains filter residue.
（3）Mass fraction is used as 0.2% dioxygen water treatment steps（2）The filter residue of collection, after washing 3 times, filter to take filter
Slag, then filter residue is placed under the conditions of 60 DEG C and dried.
（4）Take step（3）Filter residue after drying, adds EDTA solution and sodium hydroxide solution thereto, under the conditions of 30 DEG C
Stirring reaction 2 hours.
（5）Take step（4）Reacted supernatant, using the content of high performance liquid chromatography detection wherein metal ion.
Embodiment 3：A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug
A kind of technique for being used to detect metal impurities in Puerarin bulk drug, the technique comprise the following steps：
（1）The root of kudzu vine is taken, is ground into powder, 80 mesh sieves is crossed, is then immersed in 0.09mol/L hydrochloric acid solution, is handled 2 hours.
（2）To step（1）System in add 0.09mol/L sodium hydroxide solution, regulation pH value is to neutrality, then mistake
Filtrate is filtered out, obtains filter residue.
（3）Mass fraction is used as 0.2% dioxygen water treatment steps（2）The filter residue of collection, after washing 3 times, filter to take filter
Slag, then filter residue is placed under the conditions of 58 DEG C and dried.
（4）Take step（3）Filter residue after drying, adds EDTA solution and sodium hydroxide solution thereto, under the conditions of 30 DEG C
Stirring reaction 2 hours；
（5）Take step（4）Reacted supernatant, using the content of high performance liquid chromatography detection wherein metal ion.
Embodiment 4：A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug
A kind of technique for being used to detect metal impurities in Puerarin bulk drug, the technique comprise the following steps：
（1）The root of kudzu vine is taken, is ground into powder, 100 mesh sieves is crossed, is then immersed in 0.1mol/L hydrochloric acid solution, is handled 3 hours.
（2）To step（1）System in add 0.1mol/L sodium hydroxide solution, regulation pH value is to neutrality, then mistake
Filtrate is filtered out, obtains filter residue.
（3）Mass fraction is used as 0.3% dioxygen water treatment steps（2）The filter residue of collection, after washing 3 times, filter to take filter
Slag, then filter residue is placed under the conditions of 65 DEG C and dried.
（4）Take step（3）Filter residue after drying, adds EDTA solution and sodium hydroxide solution thereto, under the conditions of 35 DEG C
Stirring reaction 3 hours.
（5）Take step（4）Reacted supernatant, using the content of high performance liquid chromatography detection wherein metal ion.
Effect assessment is carried out to 1~4 technique of embodiment：
Embodiment 5：A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug
A kind of technique for being used to detect metal impurities in Puerarin bulk drug, comprises the following steps：
The first step：The root of kudzu vine is crushed, the screenings obtained after 80 mesh sieves excessively, which is immersed in hydrochloric acid solution, to be handled；
Second step：The pH value of the system of the first step is adjusted to neutrality, is then filtrated to get filter residue；
3rd step：The filter residue obtained with dioxygen water process second step, washs after terminating, filters to take filter residue, then by the filter residue
Filter residue after being dried；
4th step：EDTA solution and sodium hydroxide solution are added to the filter residue after the drying, stirring reaction 2.5 under the conditions of 27 DEG C
Hour；
5th step：The supernatant for taking the 4th step to obtain, using the content of high performance liquid chromatography detection wherein metal ion.
Preferred embodiment is：In the first step：Screenings is immersed in 0.07mol/L hydrochloric acid solutions and handled
1.5 hour.
Preferred embodiment is：In second step：Using 0.07mol/L sodium hydroxide solution, by the body of the first step
The pH value of system is adjusted to neutrality.
Preferred embodiment is：In the third step：Obtained with the dioxygen water process second step that mass fraction is 0.2%
Filter residue, it is washed with deionized after terminating 3 times.
Preferred embodiment is：In the third step：By the filter residue under the conditions of 59 DEG C, the filter after being dried
Slag.
As described above is only to explain the preferred embodiments of the invention, is not intended to tool to do any shape to the present invention
Limitation in formula, therefore all have any modification or change for making the relevant present invention under identical spirit, it should all wrap
Include the invention is intended to the category protected.
Claims (5)
- A kind of 1. technique for detecting metal impurities in Puerarin bulk drug, it is characterised in that：Comprise the following steps：The first step：The root of kudzu vine is crushed, the screenings obtained after 50~100 mesh sieves excessively, which is immersed in hydrochloric acid solution, to be handled；Second step：The pH value of the system of the first step is adjusted to neutrality, is then filtrated to get filter residue；3rd step：The filter residue obtained with dioxygen water process second step, washs after terminating, filters to take filter residue, then by the filter residue Filter residue after being dried；4th step：EDTA solution and sodium hydroxide solution are added to the filter residue after the drying, is stirred under the conditions of 25~35 DEG C anti- Answer 1~3 hour；5th step：The supernatant for taking the 4th step to obtain, using the content of high performance liquid chromatography detection wherein metal ion.
- 2. the technique according to claim 1 for detecting metal impurities in Puerarin bulk drug, it is characterised in that： In one step：Screenings, which is immersed in 0.05~0.1mol/L hydrochloric acid solutions, carries out processing 1 ~ 3 hour.
- 3. the technique according to claim 1 for detecting metal impurities in Puerarin bulk drug, it is characterised in that： In two steps：Using 0.05~0.1mol/L sodium hydroxide solution, the pH value of the system of the first step is adjusted to neutrality.
- 4. the technique according to claim 1 for detecting metal impurities in Puerarin bulk drug, it is characterised in that： In three steps：The filter residue obtained with the dioxygen water process second step that mass fraction is 0.1~0.3%, is washed with deionized after terminating 2 ~ 3 times.
- 5. the technique according to claim 1 for detecting metal impurities in Puerarin bulk drug, it is characterised in that： In three steps：By the filter residue under the conditions of 55 ~ 65 DEG C, the filter residue after being dried.
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| CN201710903565.4A CN107621510A (en) | 2017-09-29 | 2017-09-29 | A kind of pre-treating technology for being used to detect metal impurities in Puerarin bulk drug |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
Citations (2)
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| WO2011139245A1 (en) * | 2010-05-04 | 2011-11-10 | The Thailand Research Fund | A method and composition for quantifying magnesium ions |
| CN106248667A (en) * | 2016-08-23 | 2016-12-21 | 内蒙古包钢钢联股份有限公司 | A kind of Al-single crystal method in aluminium bronze |
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2017
- 2017-09-29 CN CN201710903565.4A patent/CN107621510A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011139245A1 (en) * | 2010-05-04 | 2011-11-10 | The Thailand Research Fund | A method and composition for quantifying magnesium ions |
| CN106248667A (en) * | 2016-08-23 | 2016-12-21 | 内蒙古包钢钢联股份有限公司 | A kind of Al-single crystal method in aluminium bronze |
Non-Patent Citations (2)
| Title |
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| 何蔓 等: "铈及其络合物在HPLC色谱柱上保留行为的研究——以螯合树脂及非极性柱（C8）为固定相", 《中国稀土学报》 * |
| 李登科 等: "HPLC-ICP-MS联用技术用于烟草中铬的形态分析研究", 《中国烟草学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111220692A (en) * | 2020-01-16 | 2020-06-02 | 通标标准技术服务（天津）有限公司 | Method for detecting content of heavy metal in food contact material |
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