CN109709224A - The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae - Google Patents
The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae Download PDFInfo
- Publication number
- CN109709224A CN109709224A CN201811625518.9A CN201811625518A CN109709224A CN 109709224 A CN109709224 A CN 109709224A CN 201811625518 A CN201811625518 A CN 201811625518A CN 109709224 A CN109709224 A CN 109709224A
- Authority
- CN
- China
- Prior art keywords
- iodine
- thallus laminariae
- minutes
- inorganic
- organic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The present invention relates to natural drugs to extract detection technique field, a variety of iodine can not be measured simultaneously to solve the problems, such as that conventional iodine extracts characterization processes, provide the combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae, the inorganic iodine is potassium iodide, the organic iodine is the iodo- l-tyrosine of 3- and 3, the iodo- l-tyrosine of 5- bis-, the following steps are included: accurate weigh the thallus laminariae particulate samples that 1.0g is ground, 10mL ionic liquid is added, adjusting pH value is 5.0~7.0, 15~75min is extracted in Ultrasound Instrument under the conditions of 40 DEG C of temperature, centrifugation, collect supernatant, pass through ultra performance liquid chromatography analysis detection.The present invention quickly and efficiently extracts biological active iodine by single process and using simple and relatively economical equipment using ILs as the Extraction solvent of LSE from complex sample matrix, realizes while extracting the I in detection actual sample‑, tri- kinds of inorganic and organic iodines of MIT and DIT, extraction time is short, and detection limit is low, and it is environmentally protective, and satisfied extraction efficiency can be obtained.
Description
Technical field
The present invention relates to natural drugs to extract inorganic iodine and organic iodine in detection technique field more particularly to a kind of thallus laminariae
Combined extracting detection method.
Background technique
Iodine was found in 1811 by french chemist Courtois, was naturally occurring nonmetallic member in periodic table VIIA race
Element.Iodine is most important as sound development of the required microelement to animals and humans.As thyroid hormone composition at
Point, iodine deficiency will lead to children's neurodevelopment significant delays and adult Thyroid Gland Swell and hypothyroidism.Therefore, day
The actual concentrations of different iodine substances have sizable scientific meaning in normal diet and water.In nature iodine have it is various it is inorganic and
Organic form, including iodide, iodate and organic iodine (tetraiodothyronine (T4), triiodo thryonine (T3), diiodo-
Thyronine (T2), the iodo- l-tyrosine of 3- (MIT) and 3, bis- iodo- l-tyrosine (DIT) of 5-), they may be used as diet benefit
Fill agent, catalyst, pharmaceutical preparation, stabilizer and photography applications.The measurement of iodine concentration is highly difficult in environmental and biological samples, this master
If since the concentration of iodine in sample is very low.It therefore is extremely important for measuring the analysis method of iodine using super-sensitive
's.
Currently, the main method of measurement iodine includes colorimetric method, potentiometric titration, isotope exchange method, x-ray fluorescence method
(XRF), gas chromatography (GC), high performance liquid chromatography combination Inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) and neutron
Activation analysis (NAA).In these methods, since HPLC-ICP-MS has high sensitivity, what element specificity and low detection limited
Advantage, thus be the most important method for determining iodine substance in various samples, further, since MS identification and analysis can be passed through
Object, so analyte does not need to be completely segregated.However, almost without report can pass through single process and using simply and
The equipment of relatively economical measures I simultaneously-, tri- kinds of substances of MIT and DIT, particular without the solvent extraction method for using green.
Seaweed is classified as macro, and is divided into three big groups: brown, red and green algae.Since ancient times in east
Sub- country such as Japan, South Korea and China and some western countries, including Ireland, Brittany and Wales, seaweed are foods
The important sources of product, complementary goods, drug and fertilizer.In recent years to fiber, minerals and microelement, vitamin, how unsaturated
Fatty acid, it is necessary to the research of the wholesome nutrient such as amino acid, phenols and carotenoid causes extensive concern, this
Nutrients have very strong anti-inflammatory a bit, and antibacterial is anti-oxidant, antiviral and anti-tumor activity.Since seaweed is a kind of base of complexity
Matter, it is therefore desirable to which violent operating condition and special Extraction solvent extract bioactive ingredients therein.It is deposited in seaweed
Different bioactive compounds in, iodine is important micronutrient element needed for mankind's normal thyroid function.Usually use
It include dry alkali extraction in extracting the extracting method of target iodine compound from seaweed, extraction of ocean eddies, extraction heat is microwave-assisted
Alkalinity and external digestion and microwave radiation exaraction.But these methods require a large amount of Extraction solvent and longer mention at present
Take the time.Moreover, most of sample-pretreating methods all use tetramethylammonium hydroxide (TMAH) to assess iodine at present.TMAH is
Strong basicity and if intake or skin contact be to human body it is hypertoxic, furthermore its liquid can generate nocuousness and may cause mistake
Bright toxic corrosivity steam.Therefore, it is necessary to find the substitution solvent of TMAH.
" a kind of feed in content of iodine detection method " is disclosed in Chinese patent literature, notification number is
CN104458965A, the invention have strong oxidizing property using iodate in acid condition, take under the conditions of dilute sulfuric acid, are added
Excessive Sodium Metabisulfite makes the iodine in sample all be reduced into iodide ion, then in Ion-pair HPLC solution
Iodide ion, but the invention can not detect a variety of content of iodine simultaneously.Therefore, a simple and environmentally-friendly method is developed for simultaneously
The inorganic and organic iodine measured in actual sample is significantly.
Summary of the invention
The present invention provides inorganic iodine and organic iodine in a kind of thallus laminariae to overcome above-mentioned problems of the prior art
Combined extracting detection method, using ILs as the Extraction solvent of liquid-solid extraction (LSE) for simultaneously extract in thallus laminariae it is inorganic with
Organic iodine, this method reduces the harm to human health and environment not only instead of toxic solvent, and can obtain higher
Extraction efficiency.
To achieve the goals above, the invention adopts the following technical scheme:
The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae, the inorganic iodine is potassium iodide (KI), described to have
Machine iodine is the iodo- l-tyrosine of 3- (MIT) and 3, bis- iodo- l-tyrosine (DIT) of 5-, comprising the following steps: precision weighs 1.0g mill
10mL ionic liquid is added in broken thallus laminariae particulate samples, and adjusting pH value is 5.0~7.0, in Ultrasound Instrument under the conditions of 40 DEG C of temperature
Supernatant is collected in 15~75min of middle extraction, centrifugation, passes through ultra performance liquid chromatography (UHPLC) analysis detection.
Ionic liquid (Ionic Liquid, abbreviation IL or ILs) is by specific organic cation and inorganic or organic yin
Ion composition, fusing point is equal to or less than 100 DEG C, and has been widely used as the substitution solvent of conventional organic solvents.To cation
Or hydrophobicity/the hydrophily for being suitably modified adjustable IL of anion, so as to be used according to the needs of reaction condition.
Due to its unique physics and chemical property, such as chemical stability, polarity, insignificant vapour pressure, incombustibility, low melting point,
Higher ionic conductivity, preferable thermal stability, good catalytic, wider liquidus temperature and anti-friction and wear-resistant
Property, ILs has been widely used for various fields, such as lubrication, synthesis, electrochemistry and separation and extraction field.There is presently no passes
In extracting organic and inorganic iodine compound report simultaneously from food using ILs.
The present invention develops one kind simply, and the environmental-friendly LSE method combination HPLC based on IL is planted for quantitative determining
Iodine substance in physical property food.Cheap sample pretreatment may be implemented in the combination of IL and LSE, and can ensure that and obtain satisfaction
Extraction efficiency and low detection limit.The iodo- l-tyrosine of 3- (MIT) and bis- iodo- l-tyrosine (DIT) of 3,5- are 5.0~7.0 in pH
Mainly exist in range with neutral form, the carboxyl of ionic liquid and two kinds of organic acids has strong hydrogen bond between amino and hydroxyl
It is formed, therefore pH value 5.0~7.0 is preferable extraction environment.PH value is more preferably 6.5, when the pH value of sample solution is higher than 6.5
When, the carboxyl of two kinds of organic acids, amino and hydroxyl start to dissociate, the hydrogen bond between ionic liquid and target compound is weakened,
So as to cause the reduction of target analytes extraction efficiency, therefore most preferred pH value is 6.5.
This method is easy, quickly, accurately, high sensitivity, favorable reproducibility.The present invention creatively uses ionic liquid
(ILs) substitute conventional solvent TMAH, leached simultaneously from the complex matrices such as seaweed using IL and ultrasonic wave in a water bath it is inorganic and
Organic iodine, this method does not need violent condition, and meeting is more environmentally-friendly and higher extraction is obtained within shorter extraction time
Efficiency.
Preferably, the ultra performance liquid chromatography analysis detection condition are as follows: mobile phase is by A phase and B phase composition, the A
It is mutually 10mM KH2PO4, the B phase is acetonitrile, and flow velocity is set as 0.5mL/min；Gradient elution program is as follows: 0-1 minutes, 10-
15%B；1-2 minutes, 15-25%B；2-3 minutes, 25-35%B；3-4 minutes, 35-40%B；4-5 minutes, 40-40%B；5-6
Minute, 40-45%B；6-7 minutes, 45-45%B；7-8 minutes, 45-50%B；8-9 minutes, 50-10%B；Sample volume is 2 μ L,
Detection wavelength 230nm.
The KQ-100B type ultrasonoscope (invariable power 100W) that this method is 40kHz with frequency extracts iodate from thallus laminariae
Object.The ultrasonic system is the Extracting temperature immersed in the water-bath connecting with temperature controller and needed for keeping.The elder brother ground
Cloth particulate samples are selected from the thallus laminariae sample of three kinds of different sources: Zhejiang, Fujian, the local market buying in the mountain Three Eastern Provinces.All samples
Product are dehydrating prods.The thallus laminariae particulate samples ground are fully ground by the thallus laminariae sample that is dehydrated with pulverizer powdered
Particle, and obtained after being sieved through sieve with 100 mesh stainless steels.
The method by ultra performance liquid chromatography (UHPLC) analysis detection are as follows: prepared with the reference substance of KI a series of
The reference substance solution of various concentration is detected by the similarity condition of thallus laminariae extracting solution with UHPLC, obtains the liquid chromatogram of KI reference substance
Figure is drawn the standard curve of KI using the peak area of KI chromatographic peak as ordinate, made in the same way using the concentration of KI as abscissa
Make the standard curve of MIT and DIT；According to the standard of the peak area of chromatographic peak each in the liquid chromatogram of extracting solution and each ingredient song
The content of KI, MIT and DIT in thallus laminariae extracting solution is calculated in line, and the effective component that can be accordingly calculated in extracting solution is opposite
In the content of thallus laminariae sample.
Preferably, the ionic liquid (ILs) is selected from 1- ethyl-3-methylimidazole -1- (+)-lactic acid ([Emim] [L-
L]), 1-ethyl-3-methyllimidazolium bromide ([Emim] Br), 1- butyl -3- methylimidazole mesylate ([Bmim] CH3SO3), 1-
Butyl -3- methyl imidazolium tetrafluoroborate ([Bmim] BF4), bromination 1- hexyl -3- methylimidazole ([Hmim] Br), Diethylaminoethyl
Ethyl morpholine ([Memo] Br), bromination ethylpyridine ([Epy] Br), Diethylaminoethyl ethyl piperidine ([Mepip] Br), brominated butyl
Methylpyrrole ([Bmpyr] Br), 1- dodecyl -3- methylimidazolium nitrate ([C12mim]NO3), 1- dodecyl -3- methyl
Imidazole bisulfate ([C12mim]HSO4), bromination 1- dodecyl -3- methylimidazole ([C12Mim] Br) and chlorination 1- dodecane
Base -3- methylimidazole ([C12One of mimCl).
Preferably, the ionic liquid (ILs) is bromination ethylpyridine ([EPy] Br).
As alkyl chain length increases to dodecyl, the significant reduction of extraction efficiency from ethyl.It the length of alkyl chain and is based on
Br-Ionic liquid it is related with the compatibility of water, this property will affect extraction efficiency.In addition, increasing the length of alkyl chain
It may cause the steric hindrance enhancing between extractant and target molecule, this can explain the phenomenon that total extraction efficiency declines.It examines
The influence for considering anion and cation, selects [EPy] Br as optimal extractant, this is because [EPy] Br solution has
There are stronger interaction, including π-π, ion and charge or charge are made with charge interaction and with the hydrogen bond of analyte
With.
Preferably, the concentration of the ionic liquid is 100~300mM.
Preferably, the concentration of the ionic liquid is 200mM.
Solubility and solvent extraction ability enhance with the increase of ILs concentration；However, high [EPy] Br concentration increases
The viscosity of extractant reduces a possibility that solvent penetrates into plant tissue, to reduce extraction yield.Based on above-mentioned knot
Fruit, for extracting I-, the optium concentration of the ionic liquid of MIT and DIT is 200mM.
Preferably, extraction time is 30min.
The present invention extracts in Ultrasound Instrument, and cell wall can be destroyed by extracting ultrasonic wave, therefore connecing between extracting solution and sample
Contacting surface product more increases, to make occur more target compounds in solvent.However, between upon extracting more than 30min when, peak face
The significant reduction of product.This may be since analyte is assigned in IL aqueous solution and reaches saturation in 30min.Further increase extraction
Time can cause the impurity excessively to suspend to reduce the permeability that solvent enters cell wall, and then influence to analyze in sample substrate
The extraction efficiency of object.In addition, iodide can be by oxygen in the presence of other organic compound (enzymes such as released from kelp)
It is melted into IO3 -, so that the peak area of target compound significantly reduces.Therefore, the present invention selects 30min for optimal extraction time.
Preferably, centrifugal rotational speed is 3500~4000rpm, centrifugation time is 10~15min, and more preferably centrifugation turns
Speed is 4000rpm, centrifugation time 10min.
Therefore, the invention has the following beneficial effects: lead to using ILs as the Extraction solvent of LSE instead of toxic solvent
It crosses single process and uses simple and relatively economical equipment, quickly and efficiently extract bioactivity from complex sample matrix
Iodine is realized while extracting the I in detection actual sample-, tri- kinds of inorganic and organic iodines of MIT and DIT, reduce to human health and
The harm of environment, extraction time is short, and detection limit is low, environmentally protective, and can obtain satisfied extraction efficiency.
Detailed description of the invention
Fig. 1 is the UHPLC chromatogram of the iodine standard items of three kind of 50 μ g/mL.
Fig. 2 is the UHPLC chromatogram for the thallus laminariae extracting solution that embodiment 1 originates from Shandong.
Fig. 3 is the UHPLC chromatogram for the thallus laminariae extracting solution that embodiment 2 originates from Fujian.
Fig. 4 is the UHPLC chromatogram for the thallus laminariae extracting solution that embodiment 3 originates from Zhejiang.
Specific embodiment
Below by specific embodiment, and in conjunction with attached drawing, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
The stock solution of MIT, DIT and KI are prepared with ultrapure water (18.2M Ω cm), and concentration is 200 μ g/mL, and is stored
In 4 DEG C of environment.Stock solution is diluted with water before use to prepare standard working solution.
By single factor experiment, systematic research is carried out to the several factors for influencing extraction efficiency, including extracting solution
The pH value of type and concentration, extraction time and extracting solution.The experiment of each factor carries out in triplicate, average value as a result by with
In optimization.The thallus laminariae for originating from Shandong is chosen as experiment sample, and the sample of each factors optimization is extracted simultaneously, divides immediately after
Analysis.Due to KI in thallus laminariae, the content difference of MIT and DIT are very big, so the sensitivity difference of three analytes is very big, therefore are
Convenient for observation, the two figures displayings of the result of each Optimal Parameters.
1. place of production of embodiment is the combined extracting of inorganic iodine and organic iodine detection in the thallus laminariae in Shandong:
Precision weighs the thallus laminariae particulate samples that the place of production that 1.0g is ground is Shandong and is placed in the conical flask of 50mL, is added
Bromination ethylpyridine ([EPy] Br) ionic liquid of 10mL200mM, adjusting pH value is 6.5, in ultrasound under the conditions of 40 DEG C of temperature
30min is extracted in instrument, mixture is centrifuged (4000rpm, 10 minutes), careful collection supernatant is used for ultra performance liquid chromatography
(UHPLC) it analyzes:
The chromatography of MIT, DIT and KI are carried out in 1290 ultra performance liquid chromatography of Agilent (Santa Clara, the U.S.)
's.Chromatographic column is Agilent Zorbax SB C18 column (5 μm, 4.6 × 150mm), and column temperature is maintained at 22 DEG C.Mobile phase by
10mM KH2PO4 (A) and acetonitrile (B) composition, flow velocity are set as 0.5mL/min.
Gradient elution program is as follows: 0-1 minutes, 10-15%B；1-2 minutes, 15-25%B；2-3 minutes, 25-35%B；
3-4 minutes, 35-40%B；4-5 minutes, 40-40%B；5-6 minutes, 40-45%B；6-7 minutes, 45-45%B；7-8 minutes,
45-50%B；8-9 minutes, 50-10%B.Sampling volume is 2 μ L, Detection wavelength 230nm.
Fig. 1 is the UHPLC chromatogram of the iodine standard items of three kind of 50 μ g/mL, and Fig. 2 is the thallus laminariae for originating from Shandong of the present embodiment
The UHPLC chromatogram of extracting solution obtains MIT, DIT and KI it is found that successfully extracting in gained extracting solution in conjunction with Fig. 1 and Fig. 2.
The peak area of each analyte is as shown in table 1 in the present embodiment extracting solution:
Table 1.
| Analyte | KI | MIT | DIT |
| Peak area | 6441.3 | 9.7 | 5.8 |
2. place of production of embodiment is the combined extracting of inorganic iodine and organic iodine detection in the thallus laminariae in Fujian
Embodiment 2 the difference from embodiment 1 is that, test object is the thallus laminariae that the place of production is Fujian, the complete phase of remaining process conditions
Together.
Fig. 1 is the UHPLC chromatogram of the iodine standard items of three kind of 50 μ g/mL, and Fig. 3 is the thallus laminariae for originating from Fujian of the present embodiment
The UHPLC chromatogram of extracting solution obtains MIT, DIT and KI it is found that successfully extracting in gained extracting solution in conjunction with Fig. 1 and Fig. 3.
The peak area of each analyte is as shown in table 2 in the present embodiment extracting solution:
Table 2.
| Analyte | KI | MIT | DIT |
| Peak area | 6391.3 | 9.6 | 6.0 |
3. place of production of embodiment is that the combined extracting of inorganic iodine and organic iodine detects embodiment 2 and embodiment 1 in the thallus laminariae in Zhejiang
Difference is that test object is the thallus laminariae that the place of production is Zhejiang, remaining process conditions is identical.
Fig. 1 is the UHPLC chromatogram of the iodine standard items of three kind of 50 μ g/mL, and Fig. 4 is the thallus laminariae for originating from Zhejiang of the present embodiment
The UHPLC chromatogram of extracting solution obtains MIT, DIT and KI it is found that successfully extracting in gained extracting solution in conjunction with Fig. 1 and Fig. 4.
The peak area of each analyte is as shown in table 3 in the present embodiment extracting solution:
Table 3.
| Analyte | KI | MIT | DIT |
| Peak area | 6389.3 | 9.0 | 6.3 |
Withinday precision
Precision weighs the particulate samples 1.0g ground and is placed in the conical flask of 50mL, then [EPy] Br of 10mL 200mM is molten
Liquid is added in conical flask, adjusts the pH value of sample solution to 6.5, is finally putting into temperature and is maintained in 40 DEG C of Ultrasound Instrument and extracts
30min.Later, mixture is centrifuged (4000rpm, 10 minutes), careful collection supernatant is used for ultra performance liquid chromatography
(UHPLC) it analyzes.At interior continuous sample introduction 6 times on the same day.
The relative standard deviation of the retention time of withinday precision is 0.033-0.061%, and the relative standard of peak area is inclined
Difference is 0.15-1.13%.
Day to day precision precision weighs the particulate samples 1.0g ground and is placed in the conical flask of 50mL, then by 10mL
[EPy] Br solution of 200mM is added in conical flask, is adjusted the pH value of sample solution to 6.5, is finally putting into temperature and is maintained at 40
DEG C Ultrasound Instrument in extract 30min.Later, mixture is centrifuged (4000rpm, 10 minutes), careful collection supernatant is for surpassing
High performance liquid chromatography (UHPLC) analysis.By the sample continuous sample introduction 3 days, 2 times a day.
The RSD of the peak area of the retention time of day to day precision is respectively 0.07-1.49% and 0.89-2.08%.
Repeatability is investigated referring to following experiments step, does 3 groups in parallel, is investigated as repeatability.
Precision weighs the particulate samples 1.0g ground and is placed in the conical flask of 50mL, then by [EPy] of 10mL 200mM
Br solution is added in conical flask, adjusts the pH value of sample solution to 6.5, is finally putting into temperature and is maintained in 40 DEG C of Ultrasound Instrument
Extract 30min.Later, mixture is centrifuged (4000rpm, 10 minutes), careful collection supernatant is used for ultra performance liquid chromatography
(UHPLC) it analyzes.
Medicinal material assay is accurate respectively to weigh thallus laminariae particulate samples (Zhejiang, Fujian and mountain that three kinds of different sources are ground
East) 1.0g is placed in the conical flask of 3 50mL, then [EPy] Br solution of 10mL 200mM is added in conical flask, it adjusts
The pH value of sample solution is finally putting into temperature and is maintained in 40 DEG C of Ultrasound Instrument and extract 30min to 6.5.Later, by mixture from
The heart (4000rpm, 10 minutes), careful collection supernatant are analyzed for ultra performance liquid chromatography (UHPLC).
The mixed reference substance solution that various concentration is prepared with the stock solution of KI, MIT and DIT is detected by similarity condition, is obtained
The chromatogram for obtaining three's reference substance, using the sample volume of three's reference substance as abscissa, in the chromatogram of three's reference substance solution
The peak area of chromatographic peak is ordinate, makes the standard curve of KI, MIT and DIT respectively.According to the liquid chromatogram of extracting solution and
The content of KI, MIT and DIT in three kinds of thallus laminariaes is calculated in standard curve.
Rate of recovery Assay recovery is by before extraction adding the analyte standard items of known two concentration levels
It is added in a sample (Shandong) and to be measured.Referring to following experiments step, each concentration does 3 groups of precisions in parallel and weighs mill
Broken particulate samples 1.0g is placed in the conical flask of 50mL, then [EPy] Br solution of 10mL 200mM is added to conical flask
In, the pH value of sample solution is adjusted to 6.5, is finally putting into temperature and is maintained in 40 DEG C of Ultrasound Instrument and extracts 30min.Later, will
Mixture is centrifuged (4000rpm, 10 minutes), and careful collection supernatant is analyzed for ultra performance liquid chromatography (UHPLC).
The rate of recovery is within the scope of 88-94% as shown in Table 4.Linear regression data, LOD and the LOQ of target compound and
Content, reproducibility and the rate of recovery experimental result of sample are summarized as follows table 4:
Table 4.
aAverage content value ± the standard error of every kind of compound.
The result shows that the repeatability of the method for the present invention is good, the rate of recovery is high, and detection accuracy is high.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, and is not surpassing
There are also other variations and modifications under the premise of technical solution documented by claim out.
Claims (6)
1. the combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae, which is characterized in that the inorganic iodine is iodate
Potassium, the organic iodine are the iodo- l-tyrosine of 3- and 3, the iodo- l-tyrosine of 5- bis-, comprising the following steps: precision weighs 1.0g and grinds
Thallus laminariae particulate samples, be added 10mL ionic liquid, adjust pH value be 5.0~7.0, under the conditions of 40 DEG C of temperature in Ultrasound Instrument
15~75min is extracted, supernatant is collected in centrifugation, passes through ultra performance liquid chromatography analysis detection.
2. the combined extracting detection method of inorganic iodine and organic iodine, feature exist in a kind of thallus laminariae according to claim 1
In the ultra performance liquid chromatography analysis detection condition are as follows: mobile phase is 10mM KH by A phase and B phase composition, the A phase2PO4,
The B phase is acetonitrile, and flow velocity is set as 0.5mL/min；Gradient elution program is as follows: 0-1 minutes, 10-15%B；1-2 minutes, 15-
25%B；2-3 minutes, 25-35%B；3-4 minutes, 35-40%B；4-5 minutes, 40-40%B；5-6 minutes, 40-45%B；6-7
Minute, 45-45%B；7-8 minutes, 45-50%B；8-9 minutes, 50-10%B；Sample volume is 2 μ L, Detection wavelength 230nm.
3. the combined extracting detection method of inorganic iodine and organic iodine, feature exist in a kind of thallus laminariae according to claim 1
In the concentration of the ionic liquid is 100~300mM.
4. the combined extracting detection method of inorganic iodine and organic iodine, feature exist in a kind of thallus laminariae according to claim 1
In the ionic liquid is selected from 1- ethyl-3-methylimidazole -1- (+)-lactic acid, 1-ethyl-3-methyllimidazolium bromide, 1- butyl -
3- methylimidazole mesylate, 1- butyl -3- methyl imidazolium tetrafluoroborate, bromination 1- hexyl -3- methylimidazole, Diethylaminoethyl
Ethyl morpholine, bromination ethylpyridine, Diethylaminoethyl ethyl piperidine, brominated butyl methylpyrrole, 1- dodecyl -3- methylimidazole
Nitrate, 1- dodecyl -3- methylimidazolium hydrogen sulphate salt, bromination 1- dodecyl -3- methylimidazole and chlorination 1- dodecane
One of base -3- methylimidazole.
5. the combined extracting detection method of inorganic iodine and organic iodine, feature exist in a kind of thallus laminariae according to claim 1
In extraction time 30min.
6. the combined extracting detection method of inorganic iodine and organic iodine, feature exist in a kind of thallus laminariae according to claim 1
In centrifugal rotational speed is 3500~4000rpm, and centrifugation time is 10~15min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811625518.9A CN109709224A (en) | 2018-12-28 | 2018-12-28 | The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811625518.9A CN109709224A (en) | 2018-12-28 | 2018-12-28 | The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109709224A true CN109709224A (en) | 2019-05-03 |
Family
ID=66258148
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811625518.9A Pending CN109709224A (en) | 2018-12-28 | 2018-12-28 | The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109709224A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606814A (en) * | 2020-04-28 | 2020-09-01 | 廊坊师范学院 | Ionic liquid containing citrazinic acid anions and application thereof in iodine absorption |
| CN112129862A (en) * | 2020-08-24 | 2020-12-25 | 杭州师范大学 | Method for detecting organic mercury in kelp |
| CN114894919A (en) * | 2022-04-12 | 2022-08-12 | 中国水产科学研究院黄海水产研究所 | Four iodine form liquid phase determination method based on reduction method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104435001A (en) * | 2014-11-22 | 2015-03-25 | 毛华养 | Extraction method for kelp organic iodine |
| CN106579458A (en) * | 2016-06-30 | 2017-04-26 | 天津市艾藻科技有限公司 | Refining method of seafood compound |
| CN107080223A (en) * | 2017-01-09 | 2017-08-22 | 深圳震乾坤生物科技有限公司 | Natodine powder and Natodine salt production process and its application |
-
2018
- 2018-12-28 CN CN201811625518.9A patent/CN109709224A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104435001A (en) * | 2014-11-22 | 2015-03-25 | 毛华养 | Extraction method for kelp organic iodine |
| CN106579458A (en) * | 2016-06-30 | 2017-04-26 | 天津市艾藻科技有限公司 | Refining method of seafood compound |
| CN107080223A (en) * | 2017-01-09 | 2017-08-22 | 深圳震乾坤生物科技有限公司 | Natodine powder and Natodine salt production process and its application |
Non-Patent Citations (3)
| Title |
|---|
| LI-QING PENG 等: "Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria", 《FOOD CHEMISTRY》 * |
| 国家药典委员会 编: "《中华人民共和国药典2015年版一部》", 30 June 2015, 中国医药科技出版社 * |
| 林立 等: "离子色谱-电感耦合等离子体质谱法测定植物性样品中的碘及其形态", 《色谱》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606814A (en) * | 2020-04-28 | 2020-09-01 | 廊坊师范学院 | Ionic liquid containing citrazinic acid anions and application thereof in iodine absorption |
| CN111606814B (en) * | 2020-04-28 | 2023-03-17 | 廊坊师范学院 | Ionic liquid containing citrazinic acid anions and application thereof in iodine absorption |
| CN112129862A (en) * | 2020-08-24 | 2020-12-25 | 杭州师范大学 | Method for detecting organic mercury in kelp |
| CN114894919A (en) * | 2022-04-12 | 2022-08-12 | 中国水产科学研究院黄海水产研究所 | Four iodine form liquid phase determination method based on reduction method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Altunay et al. | Monitoring of some trace metals in honeys by flame atomic absorption spectrometry after ultrasound assisted-dispersive liquid liquid microextraction using natural deep eutectic solvent | |
| Haq et al. | Deep eutectic solvent (DES) with silver nanoparticles (Ag-NPs) based assay for analysis of lead (II) in edible oils | |
| Moreda-Pineiro et al. | A review on iodine speciation for environmental, biological and nutrition fields | |
| Gómez-Ordóñez et al. | A simple ion chromatography method for inorganic anion analysis in edible seaweeds | |
| CN109709224A (en) | The combined extracting detection method of inorganic iodine and organic iodine in a kind of thallus laminariae | |
| Liu et al. | Determination of triazine herbicides in milk by cloud point extraction and high-performance liquid chromatography | |
| Romarís-Hortas et al. | Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry | |
| Calderón et al. | Perchlorate levels in soil and waters from the Atacama Desert | |
| CN103884785B (en) | A kind of detection method of selenium | |
| Peng et al. | Pyridinium ionic liquid-based liquid-solid extraction of inorganic and organic iodine from Laminaria | |
| Wang et al. | Rapid screening of mycotoxins in liquid milk and milk powder by automated size-exclusion SPE-UPLC–MS/MS and quantification of matrix effects over the whole chromatographic run | |
| Romarís-Hortas et al. | Development of anion-exchange/reversed-phase high performance liquid chromatography–inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed | |
| Akramipour et al. | Development of an efficient sample preparation method for the speciation of Se (IV)/Se (VI) and total inorganic selenium in blood of children with acute leukemia | |
| Baptista et al. | Determination of the non protein amino acid β-N-methylamino-l-alanine in estuarine cyanobacteria by capillary electrophoresis | |
| Zhang et al. | Simultaneous determination of quercetin, kaempferol, and isorhamnetin in phytopharma‐ceuticals of Hippophae rhamnoides L. by high‐performance liquid chromatography with chemiluminescence detection | |
| Gao et al. | Separation of selenium species and their sensitive determination in rice samples by ion‐pairing reversed‐phase liquid chromatography with inductively coupled plasma tandem mass spectrometry | |
| CN107677757A (en) | The method for determining vanillic aldehyde in food, methyl vanillin, Ethyl vanillin simultaneously | |
| Dong et al. | Dissipation, residues and risk assessment of metaldehyde and niclosamide ethanolamine in pakchoi after field application | |
| Buchberger | Determination of iodide and bromide by ion chromatography with post-column reaction detection | |
| Zhang et al. | Simultaneous determination of selenium containing amino acids and their sulfur-analogues in green tea and gynostemma pentaphyllum infusion with high performance liquid chromatography based on fluorescence labeling | |
| CN105510312A (en) | Orlistat rapid detection method | |
| Ge et al. | A sensitive and validated hplc method for the determination of cyromazine and melamine in herbal and edible plants using accelerated solvent extraction and cleanup with SPE | |
| Zhu et al. | Cloud point extraction and determination of trace trichlorfon by high performance liquid chromatography with ultraviolet-detection based on its catalytic effect on benzidine oxidizing | |
| Khammas et al. | Cloud point extraction of carbendazim pesticide in foods and environmental matrices prior to visible spectrophotometric determination | |
| Jouve et al. | High-performance liquid chromatography with electrochemical detection for the simultaneous determination of the methoxylated amines, normetanephrine, metanephrine and 3-methoxytyramine, in urine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190503 |
|
| RJ01 | Rejection of invention patent application after publication |