CN106908530A - IC ICP MS combinations determine method and the application of Arsenic in tea form - Google Patents
IC ICP MS combinations determine method and the application of Arsenic in tea form Download PDFInfo
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Abstract
The invention discloses method and application that a kind of IC ICP MS combinations determine Arsenic in tea form.Method and step includes 1）Tealeaves to be measured is by drying, crushing, sieving, using 0.1molL‑1Aqueous solution of nitric acid is extracted, and graphite clears up 100 DEG C of instrument and clears up 2h, obtains prepare liquid；2）Separation prepare liquid is carried out using chromatography of ions；3）Arsenic morphology is determined using CCT patterns using ICP MS.The application of described method, constitutes according to different arsenic morphologies, is applied to tea-leaf producing area and traces to the source research.Method of the present invention detection speed is fast, the degree of accuracy is high, low cost, it is adaptable to the detection of actual sample, can be used in tealeaves the accurate quantitative analysis of four kinds of arsenic morphologies and risk assessment, it is also possible to is applied to tea-leaf producing area and traces to the source research.
Description
Technical field
The present invention relates to the method that a kind of chromatography of ions-inductivity coupled plasma mass spectrometry combination determines Arsenic in tea form
And application.
Background technology
Tea is a kind of conventional beverage, in tealeaves except containing Tea Polyphenols, caffeine, vitamin etc. it is beneficial to human body it is organic into
Exceptionally, various trace elements are also contained.Trace element is beneficial to human body, and it is harmful also to have a small number of elements, it is necessary to planted
Plant to produce it is effectively monitored and controlled with process.Trace element in Accurate Determining tealeaves, for evaluating tea
Leaf quality has important meaning.
Research finds, arsenic pollution serious harm health, but arsenic to the toxicity of people and the ecosystem not only with arsenic total amount
It is relevant, it is also closely related with the chemical form that arsenic is present.In nature, the Main Morphology of arsenic has arsenate (As (V), arsenous
Hydrochlorate As (III), monomethyl arsenic (MMA), dimethyl arsenic (DMA), arsenic glycine betaine (AsB), arsenocholine (AsC) and arsenic sugar (AsS)
Deng wherein As (V), As (III) are inorganic arsenic, and other are organo-arsenic.The toxicity of inorganic arsenic is very high, there are some researches prove inorganic
Arsenic is carcinogen, and organic form arsenic is mostly nontoxic.Because the various forms of arsenic are with the different places turn all the time of local environment
Among change, so individually determining total arsenic content cannot accurately reflect the exposure level of arsenic and its influence to environment and ecology.
Therefore, the existing forms of arsenic are analyzed with measure very necessary.
In current research, the morphological research about arsenic has focused largely on soil environment, water quality, marine product and a small number of other foods
In product, wherein the Extraction solvent of arsenic compound uses methanol-water mixture or dilute acid soln mostly（Che Dong Noboru etc., Environmental Chemistry,
2014,2014,33 (7): 1130-1136）.Current professional standard《NY 659-2003》Rising limit only is done to the arsenic total amount in tealeaves
Fixed, it is current difficult point that comprehensively investigation and analysis are carried out to various arsenic morphologies in tealeaves.
The content of the invention
In order to overcome the deficiencies in the prior art, Arsenic in tea form is determined the invention provides a kind of IC-ICP-MS combinations
Method and application.
A kind of method that IC-ICP-MS combinations determine Arsenic in tea form,
1）Tealeaves to be measured is by drying, crushing, sieving, using 0.1molL-1Aqueous solution of nitric acid is extracted, and graphite clears up instrument 100
DEG C 2h is cleared up, obtain prepare liquid；
2）Separation prepare liquid is carried out using chromatography of ions；
3）Arsenic morphology is determined using CCT patterns using ICP-MS.
Described aqueous solution of nitric acid extraction conditions are specific as follows, and the g of sample 1.00 for weighing crushing clears up the 50 of instrument in graphite
In mL Teflon counteracting tanks, plus 10 mL 0.2 molL-1Salpeter solution, is mixed, and 90 DEG C are cleared up 2h, 8000 rmin-1From
The min of the heart 15, takes supernatant liquid filtering and obtains prepare liquid.
Described chromatography of ions condition：
Dionex IonPac AS7,250mm × 2mm；
Mobile phase, A is 5 molL-1 (NH4)2CO3, B is 100 molL-1 (NH4)2CO3；
Binary gradient program：0 ~ 2.5 min, 100%A；2.5 ~ 5min, 100% B；5 ~ 15min, 100% A；The mL of flow velocity 0.3
min-1, the μ L of sampling volume 25.
Described ICP-MS conditions：
The W of power 1400；
13.0 Lmin of cooling air-flow speed-1；
0.88 Lmin of secondary air speed-1；
The Lmin of flow rate of carrier gas 1.12-1；
Sampling depth 150；
Quadrupole rod biases -6.5 v；
Sextupole bar biases -8.5 v；
The v of focus voltage 9.22；
The s of acquisition time 800；
The Lmin of collision gas flow 3.0-1。
The application of described method, constitutes according to different arsenic morphologies, is applied to tea-leaf producing area and traces to the source research.
The beneficial effects of the invention are as follows the method detection speed is fast, the degree of accuracy is high, low cost, it is adaptable to actual sample
Detection, can be used in tealeaves the accurate quantitative analysis of four kinds of arsenic morphologies and risk assessment.
Due to Arsenic in tea form and the place of production（The overall situation such as including weather soil）Correlation, also adds with labor management and tealeaves
Work is relevant, it is possible to is applied to tea-leaf producing area and traces to the source research.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is that the As (III) of 20 μ g L-1, DMA, As (V) separate figure with MMA；
Fig. 2 is 4 arsenic morphology 0.5-25 μ gL-1 standard curve spectrograms.
Specific embodiment
The present invention is extracted using nitric acid, with Dionex IonPac AS7 anion-exchange columns as splitter, in correlative study
(Chungang Yuan etc. ,Food and Chemical Toxicology, 2007(45):Basis 2381-2389)
On, experimental condition is optimized, with reference to ICP-MS detections, it has been successfully set up 4 kinds of detections of main arsenic morphology in tealeaves
Method, and by the analysis to arsenic morphology in 4 teas, desk study has been made to Arsenic in tea form present situation, it is tea product kind
The research and tea leaf quality monitoring for planting arsenic Changing Pattern in process provide technical support, are the risk of arsenic in research tea product
Assessment lays the foundation.
Materials and methods
1.1 tea samples
Totally 63 samples are taken from commercially available for 4 teas, and wherein jasmine tea 10 comes from Xinjiang, and brick tea 20 takes from Hubei, green tea 18
Individual to take from Zhejiang, black tea 15 takes from Yunnan.Sample weighing, clear up before through drying, crush, sieving.
Instrument and reagent
Instrument：Thermo Fisher XSeries II type icp mses（Thermo Fisher are public in the U.S.
Department）；ICS-3000 type chromatography of ions（Thermo Fisher companies of the U.S.）；Milli-Q ultra-pure-water treatment systems（The U.S.
Millipore companies）；DEENA II samples automatically clear up preprocessing system（U.S. Thomas Cain）, IR210 rotation steamings
Hair instrument（Buchi companies of Switzerland）；Z383K type centrifuges（German Hermle companies）；KQ-100 ultrasonic cleaners（Jiangsu Province elder brother
Ultrasonic instrument Co., Ltd of mountain city）；Buchi Waterbath B-480 Rotary Evaporators（Buchi companies of Switzerland）.
Reagent：Sodium arsenite As (III), natrium arsenicum As (V), monomethyl natrium arsenicum (MMA) and dimethyl arsenate (DMA),
It is purchased from Fluka companies.Ammonium carbonate is top pure grade, Aladdin reagent Co., Ltd；Methyl alcohol and hydrogen peroxide, Merck ＆ Co., Inc.；Water is
Ultra-pure water.1.0 mgL are prepared with ultra-pure water-1Mixing As (III), DMA, MMA and As (V)（In terms of arsenic）Arsenic morphology is laid in
Liquid；Working solution is prepared using ultra-pure water stepwise dilution, matching while using.Mobile phase uses preceding de- through ultrasonic cleaner ultrasound
Gas.
Sample pre-treatments
1.2.1 the measure of arsenic total amount
G of precise 0.2 or so（It is accurate to 0.0001 g）Tea Samples add 5mL nitric acid and 1 in Teflon counteracting tank
ML hydrogen peroxide, micro-wave digestion, parameter is shown in Table 1.After clearing up end, sample is transferred in clean volumetric flask, dilution is settled to
25mL, determines for ICP-MS.
1.2.2 the measure of different shape arsenic
Arsenic morphology present in tealeaves is extracted using three kinds of pre-treating methods.
Method one：The accurate g of sample 1.00 for weighing crushing in 15 mL tool plug centrifuge tubes, plus 10 mL methanol-water
(volume ratio 1:1), mix, ultrasonic extraction 30 min, 8000 rmin-1Centrifugation 15min, takes supernatant liquid filtering.Rotary Evaporators
Filtrate is concentrated, the injury to pillar of methyl alcohol is reduced.25mL is settled to ultra-pure water, you can for the morphological analysis of arsenic.
Method two：Accurately weigh the g of sample 1.00 of crushing in 50 mL Teflon counteracting tanks, plus 10 mL 0.2
mol·L-1Salpeter solution, is mixed, and 90 DEG C are cleared up 2h, 8000 rmin-115 min are centrifuged, supernatant liquid filtering is taken.Use ultra-pure water
It is settled to 25 mL, you can for the morphological analysis of arsenic.
Method three：It is accurate to weigh the g of sample 1.00 of crushing in 50 mL Teflon counteracting tanks, add 25mL boiling water, 100
DEG C graphite clears up instrument and keeps the min of micro-boiling 30, cooling, 8000 rmin-115 min are centrifuged, supernatant liquid filtering is taken.Use ultra-pure water
It is settled to 25 mL, you can for arsenium morphological analysis in millet paste.
The preparation of mixed standard solution
4 kinds of compounds of arsenic morphology accurately are weighed, is made into containing the mgL of arsenic 1.0 with deionized water-1Mother liquor, be placed in 4 DEG C of refrigerators
In save backup.Working solution is prepared using deionized water stepwise dilution, matching while using.Mobile phase is cleaned using preceding through ultrasonic wave
Device ultrasound degassing.
Instrument condition of work
IC conditions：Dionex IonPac AS7（250mm × 2mm) anion-exchange column；Mobile phase：A is 5 molL-1
(NH4)2CO3, B is 100 molL-1 (NH4)2CO3.Binary gradient program：0 ~ 2.5 min, 100%A；2.5 ~ 5min, 100%
B；5 ~ 15min, 100% A；The mLmin of flow velocity 0.3-1, the μ L of sampling volume 25.
ICP-MS conditions：With 1.0 μ gL-1's7Li、59Co、115In、238U tuning liquid carries out instrument condition and optimizes selection,
Make 1.0 μ gL-1's115In and238The counting of U is respectively greater than 4.0 × 104Cps and 8.0 × 104Cps is carrying out total quality model
Enclose interior mass calibration.Oxide ratio CeO+/Ce+≤ 0.5%, double charge ratio B a++/Ba+≤2%；Due to35Used by Cl and instrument
High-purity carrier gas（Argon gas）Easily formed75ClAr+, interference75The measure of As, therefore, using time CCT pattern, it is used to eliminate75ClAr+Interference.The running parameter of ICP-MS is shown in Table 2 respectively.
Data processing
It is qualitative by retention time, peak area quantification.Standard curve is drawn, quantified by external standard method calculates the content of each arsenic morphology.With
Excel and SPSS 19.0 are mapped and data processing.One-way analysis of variance（Analysis of variance, ANOVA）
For comparing the difference between each group, P<0.05 represents that otherness is notable.
Result and discussion
2.1 chromatographic conditions optimize
2.1.1 mobile phase
Compare (NH4)2CO3, nitric acid:Methyl alcohol mixed solution（Volume ratio is 95:5）, nitric acid, as leacheate to As (V), As
(III), the wash-out effect of MMA, DMA.Result shows, as (NH4)2CO3During with nitric acid methyl alcohol mixed solution as mobile phase, As
(V), As (III), MMA, DMA are kept completely separate, and same concentrations nitric acid methyl alcohol mixed solution ratio (NH4)2CO3Analysis time
It is short, but As (III) and DMA separating effects are poor, and the separating effect of nitric acid is worse.Therefore, (NH is selected4)2CO3For this experiment is flowed
Phase.
Concentration and flow velocity
Analyze 1,3,5,10 mmolL-1Ammonium carbonate under given flow rate to the separating effect of As (III) and DMA, as a result
Display：With (NH4)2CO3The increase of concentration, As (III), the retention time of DMA are reduced, selection concentration 10 mmolL-1When two
Person overlaps；Select 1 mmolL-1When, As (III) has hangover serious；Select 3 mmolL-1With 5 mmolL-1When, separate
Degree is more or less the same, but appearance time significant difference, therefore 5 mmolL of selection-1 (NH4)2CO3As As (III), DMA point
From concentration.20,100,200 mmolL are investigated-1(NH4)2CO3To the separating effect of As (V) and MMA under given flow rate,
Result shows：With the increase of wash-out concentration, both appearance times shorten, but separating degree reduction, therefore selection moderate concentration
100 mmol·L-1 (NH4)2CO3As the wash-out concentration of As (V) and MMA.
Flow velocity has been respectively compared for 0.1,0.3,0.5 mLmin-1When appearance situation and post pressure, when flow velocity be 0.5
mL·min-1When, retention time is reduced, but the reduction of As (III), DMA separating degrees, and post pressure is more than 4000 psi, is unfavorable for protection
Pillar；When flow velocity is 0.1 mLmin-1When, disengaging time extension, and peak hangover is notable, therefore 0.3 mLmin of selection-1
It is this experiment optimum flow rate.
It is 0.3 mLmin to consider selection flow velocity-1, (NH4)2CO3Concentration is 5 mmolL-1With 100 mmolL-1As eluent gradient separation determination As (III), DMA, As (V) and MMA.First determine its appearance time with 4 kinds of single sample introductions of marking, then
With mixed standard solution, the peak sequence of each material is further determined that.Fig. 1 is 20 μ gL-1As (III), DMA, As (V) and
MMA separates figure, and 4 kinds of materials are relatively kept completely separate, and its retention time respectively may be about 2.08,2.92,7.34,8.03 min.
Sample extraction method optimizes
Mainly there are the reagents such as water, acid solution, methyl alcohol and enzyme currently for the Extraction solvent of arsenic morphology.This research compares 100 DEG C of water
Boil 30min, methanol-water (1:1) ultrasound 30min and 0.2 molL-190 DEG C of nitric acid aqueous solution clears up tri- kinds of extracting modes of 2h to 4 kinds of arsenic
The extraction efficiency of form.Above-mentioned three kinds put forward mode and are shown in Table 3 to the extraction effect of 4 kinds of arsenic morphologies.
As shown in Table 3, with 0.2 molL-1Aqueous solution of nitric acid is to the extraction efficiency of Arsenic in tea between 78% ~ 88%；Water is boiled
Extract minimum, no more than 50%；Methanol aqueous solution is extracted and occupy middle, between 53% ~ 68%.Because methanol aqueous solution is extracted
Afterwards, extract solution must be rotated or nitrogen blows and is eliminated as much as methyl alcohol, and to avoid the infringement to analytical column, therefore the method is relatively numerous
It is trivial.Selection is considered with 0.2 molL-1100 DEG C of aqueous solution of nitric acid clears up extracting methods of the 2h as Arsenic in tea form.
Standard working curve, detection limit and method accuracy
With optimal conditions, it is 0.5,1,5,10,25 μ gL to use stepwise dilution method to prepare mass concentration-14 kinds of arsenic series
Standard mixed solution, draws standard curve, sample concentration during using s/n=3 as instrument detection limit (LOD), during s/n=10
Sample concentration is used as instrument quantitative lower limit (LOQ).As shown in table 3,4 kinds of arsenic morphologies are in 0.5 ~ 25 μ gL for result-1In the range of be in
Good linear relationship it is good (r 2>=0.999), As (III), As (V), 4 kinds of detection limits of arsenic morphology of MMA and DMA
(LODs) 0.2,0.1,0.3,0.3 μ gL are respectively-1, lower limit of quantitation (LOQs) is respectively 0.5,0.3,0.5,0.6 μ gL-1.To 1 μ gL-1Arsenic mixed standard solution carries out the measure with relative standard deviation (RSD) in 48h in 24h, obtains 4 kinds of arsenic
RSD (n=6) is less than 4.6% less than RSD (n=3) in 4.1%, 48h in the 24h of form, and two indexs can meet routine testing need
Ask.
2.5 recovery of standard addition and method stability experiment
Under 3 mark-on levels, the rate of recovery and stability of IC-ICP-MS methods are determined, as a result as shown in table 5.4 kinds of arsenic morphologies
In 1.0,5.0 and 10.0 μ gkg-1The rate of recovery under three mark-on levels is 90.9% ~ 125.0%.Experiment is repeated 4 times, its phase
5.7% is less than to standard deviation, can be used for quantitative analysis.4 arsenic morphology 0.5-25 μ gL-1Standard curve spectrogram such as Fig. 2 institutes
Show.
As (III), the analysis result of DMA, MMA, As (V) in 2.4 tealeaves
To be separated and detected after 4 teas totally 63 sample pre-treatments, as a result shown（It is shown in Table 6-1,6-2）.63 samples
In have 7 samples and do not detect arsenic, wherein green tea 4, black tea 3.Arsenic total amount average value difference in green tea, black tea, brick tea, jasmine tea
It is 43.5,42.8,303.7,573.9 μ gkg-1, extractable total amount is respectively 38.0,38.0,285.0,509.7 μ gkg-1.Only detection As (V) in green tea, black tea has 3 samples to detect a small amount of As (III), and remaining only detects As (V), in two teas
Organic form arsenic is not detected.As (V) and As (III) is detected in brick tea and jasmine tea, and content is of a relatively high, wherein brick tea and flower
4 kinds of arsenic morphology As (III) in tea, As (DMA), As (MMA), As (V) account for correspondence extract total amount percentage be respectively 24.8%,
8.9%th, 10.2%, 56.1% and 23.1%, 7.7%, 10.0%, 59.2%.According to above-mentioned data analysis, abio-arsenic residues show in tealeaves
It is higher than organo-arsenic (P to write<0.05), and based on the As (V) of inorganic forms, content be followed successively by from high to low As (V), As (III),
MMA, DMA, the situation are similar with tobacco.
4 conclusions
Chromatography of ions-inductivity coupled plasma mass spectrometry combination analysis method that this research is set up, and to the extraction of Arsenic in tea
Method and flow visualizing are optimized, and realize being examined while As (V), As (III), tetra- kinds of arsenic morphologies of MMA and DMA in tealeaves
Survey.The method detection speed is fast, the degree of accuracy is high, it is adaptable to the detection of actual sample, while to arsenic background value in commercially available 4 teas
And 4 kinds of arsenic morphology contents have carried out initial analysis, to carry out Arsenic in tea residue detection and risk assessment provides the foundation data.
Claims (5)
1. a kind of method that IC-ICP-MS combinations determine Arsenic in tea form, it is characterized in that：
1）Tealeaves to be measured is by drying, crushing, sieving, using 0.1molL-1Aqueous solution of nitric acid is extracted, and graphite clears up 100 DEG C of instrument
2h is cleared up, prepare liquid is obtained；
2）Separation prepare liquid is carried out using chromatography of ions；
3）Arsenic morphology is determined using CCT patterns using ICP-MS.
2. method according to claim 1, it is characterized in that：Described aqueous solution of nitric acid extraction conditions are specific as follows, weigh
The g of sample 1.00 of crushing in the 50 mL Teflon counteracting tanks that graphite clears up instrument, plus 10 mL 0.2 molL-1Nitric acid is molten
Liquid, is mixed, and 90 DEG C are cleared up 2h, 8000 rmin-115 min are centrifuged, take supernatant liquid filtering and obtains prepare liquid.
3. method according to claim 1, it is characterized in that：Described chromatography of ions condition：
Dionex IonPac AS7,250mm × 2mm；
Mobile phase, A is 5 molL-1 (NH4)2CO3, B is 100 molL-1 (NH4)2CO3；
Binary gradient program：0 ~ 2.5 min, 100%A；2.5 ~ 5min, 100% B；5 ~ 15min, 100% A；The mL of flow velocity 0.3
min-1, the μ L of sampling volume 25.
4. method according to claim 1, it is characterized in that:Described ICP-MS conditions：
The W of power 1400；
13.0 Lmin of cooling air-flow speed-1；
0.88 Lmin of secondary air speed-1；
The Lmin of flow rate of carrier gas 1.12-1；
Sampling depth 150；
Quadrupole rod biases -6.5 v；
Sextupole bar biases -8.5 v；
The v of focus voltage 9.22；
The s of acquisition time 800；
The Lmin of collision gas flow 3.0-1。
5. a kind of application of method according to claim 1, it is characterized in that:Constituted according to different arsenic morphologies, be applied to tea
The leaf place of production is traced to the source research.
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| CN109030659A (en) * | 2018-09-04 | 2018-12-18 | 秦皇岛出入境检验检疫局煤炭检测技术中心 | The method of arsenic morphology in HPLC-ICP-MS combination measurement coal |
| CN109164195A (en) * | 2018-11-13 | 2019-01-08 | 浙江省海洋水产研究所 | The measuring method of inorganic arsenic in a kind of aquatic products |
| CN110987592A (en) * | 2019-12-31 | 2020-04-10 | 宁波市食品检验检测研究院 | Method for automatically and rapidly digesting food sample |
| CN111638265A (en) * | 2020-07-08 | 2020-09-08 | 中国测试技术研究院化学研究所 | Detection method for simultaneously determining bromine, iodine and phosphorus in water sample or beverage by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
| CN115356416A (en) * | 2022-09-02 | 2022-11-18 | 江苏省疾病预防控制中心(江苏省公共卫生研究院) | Method for detecting content of inorganic arsenic in tea soup |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109030659A (en) * | 2018-09-04 | 2018-12-18 | 秦皇岛出入境检验检疫局煤炭检测技术中心 | The method of arsenic morphology in HPLC-ICP-MS combination measurement coal |
| CN109164195A (en) * | 2018-11-13 | 2019-01-08 | 浙江省海洋水产研究所 | The measuring method of inorganic arsenic in a kind of aquatic products |
| CN110987592A (en) * | 2019-12-31 | 2020-04-10 | 宁波市食品检验检测研究院 | Method for automatically and rapidly digesting food sample |
| CN110987592B (en) * | 2019-12-31 | 2022-05-31 | 宁波市产品食品质量检验研究院(宁波市纤维检验所) | Method for automatically and rapidly digesting food sample |
| CN111638265A (en) * | 2020-07-08 | 2020-09-08 | 中国测试技术研究院化学研究所 | Detection method for simultaneously determining bromine, iodine and phosphorus in water sample or beverage by utilizing ICP-MS (inductively coupled plasma-mass spectrometry) |
| CN111638265B (en) * | 2020-07-08 | 2023-09-15 | 中国测试技术研究院化学研究所 | Detection method for simultaneously determining bromine, iodine and phosphorus in water sample or beverage by utilizing ICP-MS |
| CN115356416A (en) * | 2022-09-02 | 2022-11-18 | 江苏省疾病预防控制中心(江苏省公共卫生研究院) | Method for detecting content of inorganic arsenic in tea soup |
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