CN105758855A - Method for fast determining cadmium in traditional Chinese medicine materials - Google Patents
Method for fast determining cadmium in traditional Chinese medicine materials Download PDFInfo
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Abstract
The invention discloses a method for fast determining cadmium in traditional Chinese medicine materials.The method includes: crushing traditional Chinese medicine material samples, placing into a centrifugal tube, adding inorganic acid solution, performing vibrating extraction, taking filtrate, adding complex masking agent and surfactant, well mixing, and adding color developing agent for color developing so as to determine the cadmium.The method has the advantages that the method is simple to operate, accurate in determination, suitable for any sites and high in sensitivity, and the lowest detection limit of the method is 4.0microgram.L<-1>.
Description
Technical field
The invention belongs to Determination of Metals technical field, be specifically related to a kind of Cadmium detrmination method in quickly mensuration Chinese crude drug.
Background technology
Cadmium (Cadmium, Cd) is one of heavy metal that bio-toxicity is the strongest, and for chronic accumulative toxicant, Low Dose Continuous ground can accumulate gradually and present toxic action after entering body.It is generally 0.01～0.7mg kg at Cadmium in Soil constituent content-1, the growth of crop, yield and quality can be affected after entering farmland, and very easily enter animal and human's body by food chain.After entering human body, the half-life in human body, up to 6～18 years, has very strong accumulative and bioconcentration, causes that human body bone is loose, hepatic and renal function is disorderly and brings out canceration etc..According to statistics, ending global cadmium yield in 2005 and reach 100,000,000 tons, cadmium discharge capacity reaches ten thousand t more than 100, wherein about 85% enters soil, thus polluting crops.Therefore various countries have put into effect increasing regulation to control cadmium pollution problem.
The method that detection method conventional at present is mainly spot sampling, lab analysis, analysis method includes atomic absorption spectrophotometry, atomic absorption spectrophotometry, dithizone spectrophotometry, catalytic polarographic method, atomic fluorescence method, inductively coupled plasma atomic emission, inductively coupled plasma mass spectrometry etc., these methods are after sampling in test in laboratory, waiting time length and costly.In Chinese crude drug, the healthy of people is had vital impact, the foundation of cadmium method for quick, it is possible to pinpoint the problems early by the determination of cadmium content, it is to avoid harm expands further.
Summary of the invention
For solving cadmium testing cost height, time length, relying on the problems such as instrument and equipment, the present invention provides cadmium quickly to detect liquid, testing cassete and assay method, quickly detects liquid and preparation method thereof, cadmium Quick testing box and cadmium rapid assay methods including cadmium.The present invention is characterized as being with low cost, fast and easy, is independent of instrument and equipment and other compositions can be avoided measuring interference.
The present invention specifically carries and being achieved through the following technical solutions:
A kind of Chinese crude drug cadmium quick detection reagent, including screening agent, surfactant and developer, wherein said developer is that p-nitrophenyl diazoaminoazobenzene is mixed with potassium hydroxide and alcoholic solution, described surfactant is TritonX-114 solution, and described screening agent is the aqueous solution of sodium fluoride, sodium potassium tartrate tetrahydrate and thiourea composition.
Further, described developer is: weigh 50mg p-nitrophenyl diazoaminoazobenzene in the potassium hydroxide-ethanol solution of 0.3mol/L, is settled to 100mL and both obtained.
Further, described screening agent is: takes 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and is dissolved in water, is settled to 100mL and both obtained.
Further, described surfactant is: the TritonX-114 solution of 100g/L.
Present invention also offers a kind of Chinese medicine cadmium quick detection kit, this test kit includes at least three drop bottle or the container with dropper；And colorimetric card；Equipped with above-mentioned screening agent at least one of which drop bottle or container, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer.
Described Chinese medicine cadmium quick detection kit, may also include at least one cuvette or color comparison tube.Can needing to customize corresponding cuvette or color comparison tube according to mensuration, volume is about 1-50mL.
The preparation of colorimetric card: prepare the standard cadmium solution of a series of respective concentration, quickly detects the liquid reaction solution stably aobvious color of rear institute by this standard cadmium solution to cadmium and formulates corresponding colorimetric card.
Such as, the standard cadmium solution of a series of respective concentration is prepared: 4.0 μ g L-1、5.0μg·L-1、6.0μg·L-1、7.0μg·L-1、8.0μg·L-1；9.0μg·L-1、10μg·L-1、11μg·L-1、12μg·L-1、13μg·L-1、14μg·L-1、15μg·L-1Take appropriate standard cadmium solution in cuvette or color comparison tube Deng respectively, drip reagent of the present invention respectively and shake up, stand 1min, after color stability, within the color stability phase, formulate corresponding colorimetric card according to the aobvious color of institute.
A kind of Cadmium detrmination method in quickly mensuration Chinese crude drug, specifically includes following steps:
1) above-mentioned screening agent, surfactant and developer are configured；
2) dried Chinese crude drug is placed in pulverizer and is ground into granule, move in centrifuge tube, add inorganic acid solution, mechanical shaking extraction 5min, filter；
3) filtrate is placed in cuvette or color comparison tube, after dripping described screening agent, surfactant mix homogeneously, drips developer, shake up, standing, compare with colorimetric card after color stability, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
The invention have the benefit that
Being independent of instrument and equipment: do not use the instrument and equipment such as photometer, anodic stripping voltammetry electrochemical meter, visual method can realize detection；Fast and convenient: by simple operations, a few minutes can obtain result；Testing cost is low, saves cost: market common agents box (drop bottle or the container with dropper, cuvette, colorimetric card) can realize detection, and reusable；Highly sensitive: can detecting cadmium content in Chinese medicine, most mental retardation reaches 4.0 μ g L-1。
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, the following stated, it is only to presently preferred embodiments of the present invention, the present invention not does the restriction of other forms, and any those skilled in the art are changed to the equal Equivalent embodiments changed possibly also with the technology contents of the disclosure above.Every without departing from the present invention program content, any simple modification following example done according to the technical spirit of the present invention or equivalent variations, all fall within protection scope of the present invention.
The invention provides a kind of Cadmium detrmination method in quickly mensuration Chinese crude drug, after traditional Chinese medicinal material samples being pulverized, put in 5mL centrifuge tube, add 3mL inorganic acid solution, mechanical shaking extraction 5min, solution crosses 0.45 μm of filter membrane.Taking 1mL filtrate, add 1mL join masking agents, 2mL surfactant, after mixing, add 1mL chromogenic reagent, shake up, stand, compare with colorimetric card after color stability, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
Described developer is that p-nitrophenyl diazoaminoazobenzene is mixed with potassium hydroxide and alcoholic solution, and described surfactant is TritonX-114 solution, and described screening agent is the aqueous solution of sodium fluoride, sodium potassium tartrate tetrahydrate and thiourea composition.
Further, described developer is: weigh 50mg p-nitrophenyl diazoaminoazobenzene in 0.3mol L-1Potassium hydroxide-ethanol solution, be settled to 100mL both.
Further, described screening agent is: takes 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and is dissolved in water, is settled to 100mL and both obtained.
Further, described surfactant is: 100g L-1TritonX-114 solution.
Present invention also offers a kind of cadmium quick detection kit, this test kit includes at least three drop bottle or the container with dropper；And colorimetric card；Equipped with above-mentioned screening agent at least one of which drop bottle or container, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer.
Described cadmium quick detection kit, may also include at least one cuvette or color comparison tube.Can needing to customize corresponding cuvette or color comparison tube according to mensuration, volume is about 1-50mL.
The preparation of colorimetric card: prepare the standard cadmium solution of a series of respective concentration, quickly detects the liquid reaction solution stably aobvious color of rear institute by this standard cadmium solution to cadmium and formulates corresponding colorimetric card.
Such as, the standard cadmium solution of a series of respective concentration is prepared: 4.0 μ g L-1、5.0μg·L-1、6.0μg·L-1、7.0μg·L-1、8.0μg·L-1；9.0μg·L-1、10μg·L-1、11μg·L-1、12μg·L-1、13μg·L-1、14μg·L-1、15μg·L-1Take appropriate standard cadmium solution in cuvette or color comparison tube Deng respectively, drip reagent of the present invention respectively and shake up, stand 1min, after color stability, within the color stability phase, formulate corresponding colorimetric card according to the aobvious color of institute.
Embodiment 1
1) different sources Radix Salviae Miltiorrhizae is chosen as traditional Chinese medicine sample, sample details such as table 1.
The Radix Salviae Miltiorrhizae of table 1 different sources
Produce testing sample:
Respectively by dried Radix Salviae Miltiorrhizae 1#, Radix Salviae Miltiorrhizae 2#, Radix Salviae Miltiorrhizae 3#It is placed in pulverizer and is ground into granule, move in centrifuge tube, add inorganic acid solution, mechanical shaking extraction 5min, be filtrated to get filtrate, respectively filtrate 1#, filtrate 2#, filtrate 3#, correspond to Radix Salviae Miltiorrhizae 1#, Radix Salviae Miltiorrhizae 2#, Radix Salviae Miltiorrhizae 3#。
2) cadmium quick detection reagent
Developer: weigh 50mg p-nitrophenyl diazoaminoazobenzene in 0.3mol L-1Potassium hydroxide-ethanol solution, be settled to 100mL both.
Screening agent: take 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and be dissolved in water, is settled to 100mL and both obtained.
Surfactant: 100g L-1TritonX-114 solution.
3) preparation of colorimetric card:
Prepare 4.0 μ g L-1、5.0μg·L-1、6.0μg·L-1、7.0μg·L-1、8.0μg·L-1；9.0μg·L-1、10μg·L-1、11μg·L-1、12μg·L-1、13μg·L-1、14μg·L-1、15μg·L-1Cadmium standard solution, take 12 cuvette (capacity 5-15mL, and with 5mL graduation mark) add above-mentioned solution and be about 5mL to 5mL scale, after dripping described screening agent, surfactant mix homogeneously respectively, dropping developer, shakes up, and stands 1min, after color stability, within the color stability phase, formulate corresponding colorimetric card according to the aobvious color of institute.
4) sample determination
Adopt above-mentioned cuvette, cuvette is rinsed 1～3 time with filtrate to be measured, cuvette takes water sample to be measured to 5mL graduation mark, in cuvette water sample to be measured, drip screening agent and surfactant shakes up, drip developer again and stand 1min, then cuvette being pressed close to the gutter of colorimetric card, by liquid color in cuvette compared with colour code portion color, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
5) sample determination result
The inventive method and flame atomic absorption spectrometry contrast, result is in Table 2.
Table 2
By data in table 2 it can be seen that when detecting Radix Salviae Miltiorrhizae, method for quick of the present invention is almost identical with flame atomic absorption spectrometry, and has simple and quick feature.
Embodiment 2
1) the different sources Radix Aucklandiae is chosen as traditional Chinese medicine sample, sample details such as table 1.
The Radix Aucklandiae of table 1 different sources
Produce testing sample:
Respectively by the dried Radix Aucklandiae 1#, the Radix Aucklandiae 2#, the Radix Aucklandiae 3#It is placed in pulverizer and is ground into granule, move in centrifuge tube, add inorganic acid solution, mechanical shaking extraction 5min, be filtrated to get filtrate, respectively filtrate 1#, filtrate 2#, filtrate 3#, correspond to the Radix Aucklandiae 1#, the Radix Aucklandiae 2#, the Radix Aucklandiae 3#。
2) cadmium quick detection reagent
Developer: weigh 50mg p-nitrophenyl diazoaminoazobenzene in 0.3mol L-1Potassium hydroxide-ethanol solution, be settled to 100mL both.
Screening agent: take 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and be dissolved in water, is settled to 100mL and both obtained.
Surfactant: 100g L-1TritonX-114 solution.
3) preparation of colorimetric card:
Prepare 4.0 μ g L-1、5.0μg·L-1、6.0μg·L-1、7.0μg·L-1、8.0μg·L-1；9.0μg·L-1、10μg·L-1、11μg·L-1、12μg·L-1、13μg·L-1、14μg·L-1、15μg·L-1Cadmium standard solution, take 12 cuvette (capacity 5-15mL, and with 5mL graduation mark) add above-mentioned solution and be about 5mL to 5mL scale, after dripping described screening agent, surfactant mix homogeneously respectively, dropping developer, shakes up, and stands 1min, after color stability, within the color stability phase, formulate corresponding colorimetric card according to the aobvious color of institute.
4) sample determination
Adopt above-mentioned cuvette, cuvette is rinsed 1～3 time with filtrate to be measured, cuvette takes water sample to be measured to 5mL graduation mark, in cuvette water sample to be measured, drip screening agent and surfactant shakes up, drip developer again and stand 1min, then cuvette being pressed close to the gutter of colorimetric card, by liquid color in cuvette compared with colour code portion color, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
6) sample determination result
The inventive method and flame atomic absorption spectrometry contrast, result is in Table 2.
Table 2
By data in table 2 it can be seen that when detecting the Radix Aucklandiae, method for quick of the present invention is almost identical with flame atomic absorption spectrometry, and has simple and quick feature.
Embodiment 3
1) different sources Rhizoma Corydalis is chosen as traditional Chinese medicine sample, sample details such as table 1.
The Rhizoma Corydalis of table 1 different sources
Produce testing sample:
Respectively by dried Rhizoma Corydalis 1#, Rhizoma Corydalis 2#, Rhizoma Corydalis 3#It is placed in pulverizer and is ground into granule, move in centrifuge tube, add inorganic acid solution, mechanical shaking extraction 5min, be filtrated to get filtrate, respectively filtrate 1#, filtrate 2#, filtrate 3#, correspond to Rhizoma Corydalis 1#, Rhizoma Corydalis 2#, Rhizoma Corydalis 3#。
2) cadmium quick detection reagent
Developer: weigh 50mg p-nitrophenyl diazoaminoazobenzene in 0.3mol L-1Potassium hydroxide-ethanol solution, be settled to 100mL both.
Screening agent: take 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and be dissolved in water, is settled to 100mL and both obtained.
Surfactant: 100g L-1TritonX-114 solution.
3) preparation of colorimetric card:
Prepare 4.0 μ g L-1、5.0μg·L-1、6.0μg·L-1、7.0μg·L-1、8.0μg·L-1；9.0μg·L-1、10μg·L-1、11μg·L-1、12μg·L-1、13μg·L-1、14μg·L-1、15μg·L-1Cadmium standard solution, take 12 cuvette (capacity 5-15mL, and with 5mL graduation mark) add above-mentioned solution and be about 5mL to 5mL scale, after dripping described screening agent, surfactant mix homogeneously respectively, dropping developer, shakes up, and stands 1min, after color stability, within the color stability phase, formulate corresponding colorimetric card according to the aobvious color of institute.
4) sample determination
Adopt above-mentioned cuvette, cuvette is rinsed 1～3 time with filtrate to be measured, cuvette takes water sample to be measured to 5mL graduation mark, in cuvette water sample to be measured, drip screening agent and surfactant shakes up, drip developer again and stand 1min, then cuvette being pressed close to the gutter of colorimetric card, by liquid color in cuvette compared with colour code portion color, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
7) sample determination result
The inventive method and flame atomic absorption spectrometry contrast, result is in Table 2.
Table 2
By data in table 2 it can be seen that when detecting Rhizoma Corydalis, method for quick of the present invention is almost identical with flame atomic absorption spectrometry, and has simple and quick feature.
Claims (6)
1. Cadmium detrmination method in a quick mensuration Chinese crude drug, it is characterised in that comprise the following steps:
1) configuration screening agent, surfactant and developer；
2) dried Chinese crude drug is placed in pulverizer and is ground into granule, move in centrifuge tube, add inorganic acid solution, mechanical shaking extraction 5min, filter；
3) filtrate being placed in cuvette or color comparison tube, after dropping screening agent, surfactant mix homogeneously, drip developer, shake up, stand, compare with colorimetric card after color stability, numerical value shown in the immediate colour code of color is tested Chinese medicine cadmium content.
2. assay method according to claim 1, it is characterised in that
Described developer is that p-nitrophenyl diazoaminoazobenzene is mixed with potassium hydroxide and alcoholic solution；
Described surfactant is TritonX-114 solution；
Described screening agent is the aqueous solution of sodium fluoride, sodium potassium tartrate tetrahydrate and thiourea composition.
3. assay method according to claim 2, it is characterised in that
Described developer is: weigh 50mg p-nitrophenyl diazoaminoazobenzene in 0.3mol L-1Potassium hydroxide-ethanol solution, be settled to 100mL both；
Described screening agent is: takes 5g sodium fluoride, 5g sodium potassium tartrate tetrahydrate and 6g thiourea and is dissolved in water, is settled to 100mL and both obtained；
Described surfactant is: 100g L-1TritonX-114 solution.
4. a Chinese medicine cadmium quick detection kit, it is characterised in that this test kit includes at least three drop bottle or the container with dropper；And colorimetric card；
Equipped with above-mentioned screening agent at least one of which drop bottle or container, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer, at least one drop bottle or with in the container of dropper equipped with above-mentioned developer.
5. test kit according to claim 4, it is characterised in that described Chinese medicine cadmium quick detection kit, also includes at least one cuvette or color comparison tube.
6. test kit according to claim 5, it is characterised in that described colorimetric card, by preparing the standard cadmium solution of a series of respective concentration, quickly detects liquid reaction solution stably rear aobvious color by this standard cadmium solution and cadmium and prepares.
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| CN201610254913.5A CN105758855A (en) | 2016-04-22 | 2016-04-22 | Method for fast determining cadmium in traditional Chinese medicine materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106526072A (en) * | 2016-11-24 | 2017-03-22 | 宁德师范学院 | Cd<2+> one-step detection preformed reagent and method |
| CN107247049A (en) * | 2017-06-12 | 2017-10-13 | 天津科技大学 | The test paper of cadmium content in a kind of detection cereal with screening agent |
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| JPS54141196A (en) * | 1978-04-25 | 1979-11-02 | Matsushita Electric Ind Co Ltd | Measuring apparatus for concentration of very slight amount of cadmium ions |
| CN103323453A (en) * | 2013-06-26 | 2013-09-25 | 北京桑普生物化学技术有限公司 | Rapid detection solution, kit and detection method for cadmium |
| CN103776822A (en) * | 2013-09-12 | 2014-05-07 | 天津凯英科技发展有限公司 | Rapid heavy-metal detection method, as well as test paper and preparation method thereof |
| CN103776826A (en) * | 2014-01-16 | 2014-05-07 | 无限极（中国）有限公司 | Masking-agent-containing test strip for detecting content of cadmium in Chinese herbal medicine |
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2016
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| JPS54141196A (en) * | 1978-04-25 | 1979-11-02 | Matsushita Electric Ind Co Ltd | Measuring apparatus for concentration of very slight amount of cadmium ions |
| CN103323453A (en) * | 2013-06-26 | 2013-09-25 | 北京桑普生物化学技术有限公司 | Rapid detection solution, kit and detection method for cadmium |
| CN103776822A (en) * | 2013-09-12 | 2014-05-07 | 天津凯英科技发展有限公司 | Rapid heavy-metal detection method, as well as test paper and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106526072A (en) * | 2016-11-24 | 2017-03-22 | 宁德师范学院 | Cd<2+> one-step detection preformed reagent and method |
| CN107247049A (en) * | 2017-06-12 | 2017-10-13 | 天津科技大学 | The test paper of cadmium content in a kind of detection cereal with screening agent |
| CN107247049B (en) * | 2017-06-12 | 2019-09-03 | 天津科技大学 | A kind of test paper for detecting cadmium content in cereal with screening agent |
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