CN102539606B - Determination method of trivalent aluminum in aquatic product and product thereof - Google Patents
Determination method of trivalent aluminum in aquatic product and product thereof Download PDFInfo
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Abstract
The invention discloses a determination method of trivalent aluminum in an aquatic product and a product thereof. The determination method comprises the following steps: extracting trivalent aluminum in the aquatic product and the product thereof by using a mixed liquid of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid and 0.090mol/L glacial acetic acid; separating in a high performance liquid chromatograph; eluting Al in various forms with a flowing phase sequentially because a cation-exchange chromatographic column has different absorption capabilities on Al in various forms; analyzing and detecting 27AL in an eluent through an inductive coupling plasma spectrometer, thus more complete biological characteristics of Al in the aquatic product are given. According to the invention, the experiment conditions are reasonably selected, and the detection data is accurate and reliable and is not influenced by digestion time and temperature; and by using the method, the contents of trivalent aluminum in the aquatic product and the product thereof can be determined accurately.
Description
Technical field:
The invention belongs to the aquatic products detection technique, relate to particularly a kind of method of measuring trivalent aluminium in aquatic products and goods thereof with high performance liquid chromatography-Inductively coupled plasma mass spectrometry (HPLC-ICP-MS) coupling technique.
Background technology:
Current, a forward position content of elementary analytical chemistry is that the different shape to element carries out quantitative and qualitative analysis, and be not only the total amount of measuring element, this is mainly because the different shape of identity element may have diverse chemical property, aluminium is one of them typical element.The chemical form of aluminium element in the hydrobionts such as marine alga is different from terrestrial organism, and element morphology difference is to affect the key factor that the marine alga edible safety is estimated, but the research of this respect is less, and particularly relevant marine alga aspect is close to blank.
Find according to up-to-date research, in physical environment and living things system, aluminium has variform, and the toxicity of different shape aluminium differs greatly.Result of study shows that there is variform in Aluminum in Aquatic Products, mainly with stable, organo-aluminium form that be difficult for being absorbed by biosome, exist, and higher inorganic states aluminium (trivalent aluminium) content of toxicity is lower.About aquatic products processes such as process washing, the cooking in edible process, whether form and the content of the aluminium in body have changed, and the research final conclusion is also not yet arranged in addition.
The detection method of existing aluminium is: the assay method of aluminium in the flour-made food of stipulating in GB GB/T5009.182-2003, and the algae such as sea-tangle, laver are by the photosynthesis self-sow in breeding process, it is a kind of marine food of pure natural, the processing of the product such as sea-tangle, laver is generally through washing dish, dehydration, moulding, oven dry, packs, weighs and the flow process such as storage, especially there is no need to add leavening agent aluminium potassium sulfate (potassium alum) and alum (ammonia-alum) in process, the processing of this and Flour product or dilated food is diverse.Therefore, the Aluminium residual that adopts the method to detect marine alga and the aquatic products take marine alga as the Major Foods chain and goods thereof all exceed standard ((mg/kg)≤100 of limiting the quantity of of aluminium in food additives hygienic standard GB2760-2007).Aluminium in aquatic products is not the aluminium potassium sulfate of GB2760 indication or the trivalent aluminium in Exsiccated Ammonium Alum fully---" non-those aluminium of this aluminium ".Therefore extremely urgent to research and the foundation of Aluminum in Aquatic Products morphological analysis method, become the important front edge problem that the National Nature scientific basic develops.As early as possible the assay method of trivalent aluminium is studied, and set up and to be suitable for the standard method that all kinds of aquatic products detect and to be very important.There is no the method standard of measuring trivalent aluminium in aquatic products in present international ISO and CAC standard.
Summary of the invention:
The technical problem to be solved in the present invention is to provide the assay method of trivalent aluminium in a kind of aquatic products and goods thereof, use high performance liquid chromatography-Inductively coupled plasma mass spectrometry coupling (HPLC-ICP-MS) Valence Analysis, form to its trivalent aluminium is carried out qualitative and quantitative analysis, trivalent aluminium in Accurate Determining aquatic products and goods thereof, thus biological characteristics more accurately and reliably provided.
The present invention completes according to following method of operating:
The assay method of trivalent aluminium in a kind of aquatic products and goods thereof, comprise the following steps: the instrument of 1, selecting and equipment, HPLC-ICP-MS combined system, 2, configuration reagent and standard solution, 3, the step of sample preparation, 4, experiment instrument condition 5 used, sample detection and result calculating; Concrete steps are as follows:
1) instrument of selecting and equipment, the HPLC-ICP-MS combined system:
(1), HPLC part: use SERIES200 high pressure liquid phase pump, be furnished with automatic sampler, be furnished with CG5A 4 * 250mm cation-exchange chromatography post of guard column CG5A 4 * 50mm and identical material filler;
(2), ICP-MS: be furnished with Dynamic Reaction Cell, sampling system, radio-frequency signal generator, plasma system, interface, ion lens system, quadrupole rod, vacuum system, detecting device, air-path control system;
(3), cooling circulating water;
(4), water-bath constant temperature oscillator;
(5), sand core filter;
(6), circulating vacuum pump;
(7), hydro-extractor;
(8), numerical control ultrasonic cleaning machine;
(9), the water system miillpore filter of 0.45 μ m;
(10), the argon gas of purity 〉=99.99%;
2) configuration reagent and standard solution:
(1), leaching liquor: the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid;
(2), mobile phase: the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid, before using through 0.45 μ m membrane filtration and ultrasonic degas;
All reagent is all that analysis is pure or top grade is pure, and ultrapure water is all used in whole experiment; Glass apparatus uses front through 15% nitric acid dousing 24h;
(3), the standard solution of AL (III):
AL (III) standard solution: the storing solution that 100 μ g/mL AL (III) standard solution is diluted to 1.00 μ g/mL AL (III), putting 4 ℃ of refrigerators deposits standby, AL (III) storing solution by 1.00 μ g/mL is diluted to AL (III) standard solution of 50.0ng/mL, 100.0ng/mL, 250.0ng/mL, 500.0ng/mL, 1000.0ng/mL, matching while using through mobile phase;
3) step of sample preparation:
Dry sample 0.400g～the 0.800g that takes through pulverizing 40 mesh sieves is placed in 50mL tool plug scale test tube, adding extract 20mL mixes, or bright sample smashs homogenate to pieces and takes 2.000g～4.000g and be placed in 50mL tool plug scale test tube, adds extract 20mL and mixes, to 70 ℃ of water bath with thermostatic control shaking table 1h, after the abundant lixiviate of sample, take out coolingly, the centrifugal 15min of 4000r/min, take out supernatant with the water system filtering with microporous membrane of 0.45 micron, move in sample injection bottle, upper machine is measured the value of trivalent aluminium;
4) experiment instrument condition used:
(1), high-efficient liquid phase chromatogram condition HPLC: mobile phase is the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid, flow velocity 1mL/min; Sampling volume 50～100 μ L, auto injection;
(2), Inductively coupled plasma mass spectrometry condition ICP-MS: radio-frequency power 1150～1600W, plasma flow speed 15～20L/min, assisted gas flow velocity 1.2～1.5L/min; Sampling time 10min; Measure mass number
27AL;
5) sample detection and result are calculated:
(1), qualitative: as to arrange by above-mentioned condition after start, after stable, first do typical curve, then measure the sample measuring liquid for the treatment of of handling well; Adopt full-automatic injector sample introduction 50～100 μ L to measure under above-mentioned high performance liquid chromatography and Inductively coupled plasma mass spectrometry condition, high performance liquid chromatograph separates, Inductively coupled plasma mass spectrometry pair
27AL detects; Trivalent aluminium AL (III) retention time is about 3.172min under above-mentioned instrument condition;
(2), quantitative: the chromatographic peak retention time for the treatment of AL in sample measuring liquid (III) is compared variation range and namely think this material to be determined within ± 10% with standard solution;
Result is calculated and statement
With the external standard method in data processing software, determine AL (III) retention time and degree of separation pulse strength, take concentration as horizontal ordinate, the pulse strength integration is ordinate, the drawing standard working curve,, then with sample liquid peak analyzing and processing, can obtain treating the concentration of the AL (III) in sample measuring liquid, calculate the content of trivalent aluminium in derived sample by following formula (1):
X＝C×V/m×1000............... (1)
In formula:
The content of trivalent aluminium in the X-sample, mg/kg;
C-treats the concentration of trivalent aluminium in sample measuring liquid, ng/ml;
The m-sample weighting amount, g;
V-measures total liquid volume, mL.
The present invention's beneficial effect compared with prior art is:
1, after the AL (III) in aquatic products and goods thereof extracts with extract, separate by high performance liquid chromatograph, because the cation-exchange chromatography post is different to the adsorptive power of the various forms of Al, mobile phase is with its wash-out successively, and eluent is through Inductively coupled plasma mass spectrometry pair
27AL carries out analyzing and testing, and this choice of experimental conditions is reasonable, detects data accurately and reliably.
2, in the inventive method mensuration aquatic products sample and goods thereof, the form of AL (III) is not affected by extraction time and temperature, the content of AL (III) in energy Accurate Determining aquatic products and goods thereof.
3, the present invention has filled up in present GB the blank that total aluminium assay method is only arranged and AL (III) form detection method is not arranged, the evaluation aquatic products of energy accurate science and the quality of goods thereof.
Description of drawings:
Fig. 1: AL (III) standard solution form spectrogram;
Fig. 2: the sea-tangle sample is lixiviate 0.5～2.0h AL (III) form spectrogram in 70 ℃ of waters bath with thermostatic control;
Embodiment:
Describe technology contents of the present invention in detail below by embodiment:
The present invention is for utilizing the morphological analysis method of high performance liquid chromatography-Inductively coupled plasma mass spectrometry coupling (HPLC-ICP-MS) Valence Analysis to trivalent aluminium in aquatic products and goods thereof, step comprises: the instrument of 1, selecting and equipment, 2, configuration reagent and standard solution, 3, the step of sample extraction, 4, experiment instrument condition used, 5, sample detection and result calculating.
Aquatic products are various in style, as shellfish, fish, shell-fish, siphonopods and various algae etc.; Inrichment and mechanism to aluminium in its growth course are different, in its body, content and the existence form of aluminium also differ greatly, the chemical form of aluminium element in the hydrobionts such as marine alga is different from terrestrial organism, element morphology difference is to affect the key factor that the marine alga edible safety is estimated, this to be present in different biosomes and algae in the mensuration of aluminium have higher requirement, especially with algae for very.Therefore, we select the embodiment of the algae of the most representative in aquatic products and dispute maximum as checking.
Embodiment 1: the mensuration of AL in sea-tangle (III)
1, instrument and the equipment selected of the present embodiment: HPLC-I CP-MS combined system:
(1), HPLC (U.S. Perkin-Elmer company, model Series 200) part: use SERIES200 high pressure liquid phase pump, be furnished with automatic sampler, be furnished with CG5A 4 * 250mm cation-exchange chromatography post of guard column CG5A 4 * 50mm and identical material filler;
(2), ICP-MS (U.S. Perkin-Elmer company, model ELAN DRCII) part: be furnished with Dynamic Reaction Cell (DRC), sampling system, radio-frequency signal generator, plasma system, interface, ion lens system, quadrupole rod, vacuum system, detecting device, air-path control system;
(3), cooling circulating water (U.S. POLYSCIENCE company, model SHA-C);
(4), water-bath constant temperature oscillator (Shanghai and glad instrument and meter company limited, model SHA-C);
(5), sand core filter (core filtration unit, model SH/T0093);
(6), circulating vacuum pump (Shanghai Yarong Biochemical Instrument Plant, model SHZ-III);
(7), hydro-extractor (Beijing Lei Boer hydro-extractor company limited, model LD5-10);
(8), numerical control ultrasonic cleaning machine (some company of city of Kunshan's ultrasonic instrument, model KQ-600DE);
(9), water system miillpore filter (0.45 μ m);
(10), argon gas (purity 〉=99.99%).
2, configuration reagent and standard solution;
(1), leaching liquor takes lithium hydroxide 1.700g, pyridine-2.6-dicarboxylic acid 1.000g, glacial acetic acid 5.420g, slowly be settled to 1000mL with ultrapure water, obtain the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid after mixing.
(2), mobile phase: the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid.Use front through 0.45 μ m membrane filtration and ultrasonic degas.
All reagent is all that analysis is pure or top grade is pure, and ultrapure water is all used in whole experiment; Glass apparatus uses front through 15% nitric acid dousing 24h;
(3), the standard solution of AL (III):
AL (III) standard solution: buy the standard solution of 100 μ g/mLAL (III) from State center for standard matter, be diluted to the storing solution (put 4 ℃ refrigerators deposit standby) of 1.00 μ g/mL as AL (III); 1.00 the AL of μ g/mL (III) storing solution is diluted to AL (III) standard solution of 50.0ng/mL, 100.0ng/mL, 250.0ng/mL, 500.0ng/mL, 1000.0ng/mL, matching while using through mobile phase.
3, the step of sample preparation:
Take through pulverizing 40 mesh sieves dry sample approximately 0.400g be placed in 50mL tool plug scale test tube, 20mL mixes with leaching liquor,, to 70 ℃ of water bath with thermostatic control shaking table 1h, after the abundant lixiviate of sample, takes out cooling.The centrifugal 15min of 4000r/min, take out supernatant with the water system filtering with microporous membrane of 0.45 micron, moves in sample injection bottle the value of upper machine mensuration trivalent aluminium.
4, experiment instrument condition used;
(1), high-efficient liquid phase chromatogram condition HPLC: the mixed liquor of mobile phase 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid, flow velocity 1mL/min; Sampling volume 50 μ L, auto injection.
(2), Inductively coupled plasma mass spectrometry condition ICP-MS: radio-frequency power 1150W, plasma flow speed 15L/min, assisted gas flow velocity 1.2L/min; Sampling time 10min.Measure mass number
27AL.
5, sample detection and result are calculated:
(1), qualitative: as to arrange by above-mentioned condition after start, after stable, first do typical curve, then measure the sample solution of handling well.Adopt full-automatic injector sample introduction 50 μ L to measure under above-mentioned high performance liquid chromatography and Inductively coupled plasma mass spectrometry condition, high performance liquid chromatograph separates, Inductively coupled plasma mass spectrometry pair
27AL detects; Trivalent aluminium AL (III) retention time is about 3.172min under above-mentioned instrument condition; See Fig. 1 for details;
(2), quantitative: the chromatographic peak retention time of AL in testing sample (III) is compared variation range and namely think this material to be determined within ± 10% with standard solution;
Result is calculated and statement
With the external standard method in data processing software (chromera), determine AL (III) retention time and degree of separation pulse strength, take concentration as horizontal ordinate, the pulse strength integration is ordinate, and the drawing standard working curve is preserved standard working curve, then with sample peak analyzing and processing, can obtain treating the concentration of the AL (III) in sample measuring liquid, by following formula (1), calculate, can obtain the content of trivalent aluminium in sample:
X＝C×V/m×1000............... (1)
In formula:
The content of trivalent aluminium in the X-sample, mg/kg;
C-treats the concentration of AL in sample measuring liquid (III), ng/ml;
The m-sample weighting amount, g;
V-measures total liquid volume, mL;
6, result and discussion:
The analytical performance of table 2, instrument
As shown in Table 2: the analytical performance of this instrument meets fully measures Al (III);
The measurement result of table 3, sea-tangle recovery of standard addition (in butt):
As shown in Table 3: we add target Al (III) recovery 88.7%, and recovering effect is desirable.
For our measure taked accurately and reliably of guaranteeing experimental data has: 1. sample need be pulverized 40 mesh sieves and can make like this sample even, and lixiviate is (in Table 3) fully; 2. select the leaching liquor of research screening can make between al species to sea-tangle and do not cause interference, Al (III) is extracted fully; 3., guard column CG5A 4 * 50mm of selecting, CG5A 4 * 250mm cation exchange column can make al species separate to see Fig. 2.By this spectrogram as can be known: 1. the form of sample Al after extract extracts does not change along with the increase of extraction time.2. the peak shape of AL (III) is highly stable, proves between al species and can mutually not transform with the increase of extraction time.
Embodiment 2: to the mensuration of Al in sea cucumber (III):
Take bright sample (need smash homogenate to pieces) 4.000g and be placed in 50mL tool plug scale test tube, add mobile phase 20mL and mix., to 70 ℃ of shaking bath 1h, make the abundant lixiviate of sample.Take out cooling.The centrifugal 15min of 4000r/min, take out supernatant with the water system filtering with microporous membrane of 0.45 micron, the value of upper machine mensuration AL (III).Other condition is identical with sea-tangle all, the measurement result of sea cucumber recovery of standard addition (in Table 4).
The measurement result of table 4, sea cucumber recovery of standard addition (in butt)
As shown in Table 4: we add the recovery of target Al (III) 90.1%, and recovering effect is desirable;
In sum, as shown in Table 2: the analytical performance of this instrument meets the requirement of measuring AL (III) fully, by table 3 and table 4 as can be known we add target Al (III) the recovery at 88.7%-90.1%, recovering effect is desirable.This pre-treatment that has benefited from instrument that we select and instrument condition, extract concentration, sample very rationally puts in place.The bright spot of the method: the Al in aquatic products and goods thereof (III) is after extract extracts, separate by high performance liquid chromatograph, because the cation-exchange chromatography post is different to the adsorptive power of the various forms of Al, mobile phase is with its wash-out successively, and eluent is through Inductively coupled plasma mass spectrometry pair
27AL carries out analyzing and testing; This method detection line is low, and sensitivity, accuracy are high;
Therefore want to measure accurately the Al (III) in aquatic products and goods thereof, must use high performance liquid chromatography-Inductively coupled plasma mass spectrometry coupling (HPLC-ICP-MS) morphological analysis method.This method has provided aluminium in the more complete biological characteristics of the aluminium in aquatic products, particularly current marine alga and has measured and to have caused in the situation of dispute in many ways, and adopting more clear, the morphological analysis of HPLC-HGAFS coupling accurately is best first-selection.We are just presiding over the formulation of bearing China's agricultural industry criteria " assay method of trivalent aluminium and organo-aluminium in marine alga and goods thereof " at present, with it, fill up in ISO and CAC standard and there is no this blank of detection method of measuring trivalent aluminium in aquatic products and goods thereof.
Claims (1)
1. the assay method of trivalent aluminium in aquatic products and goods thereof, comprise the following steps: the instrument of 1, selecting and equipment, HPLC-ICP-MS combined system, 2, configuration reagent and standard solution, 3, the step of sample preparation, 4, experiment instrument condition 5 used, sample detection and result calculating; It is characterized in that concrete steps are as follows:
1) instrument of selecting and equipment, the HPLC-ICP-MS combined system:
(1), HPLC part: use SERIES200 high pressure liquid phase pump, be furnished with automatic sampler, be furnished with the CG5A4 of guard column CG5A4 * 50mm and identical material filler * 250mm cation-exchange chromatography post;
(2), ICP-MS: be furnished with Dynamic Reaction Cell, sampling system, radio-frequency signal generator, plasma system, interface, ion lens system, quadrupole rod, vacuum system, detecting device, air-path control system;
(3), cooling circulating water;
(4), water-bath constant temperature oscillator;
(5), sand core filter;
(6), circulating vacuum pump;
(7), hydro-extractor;
(8), numerical control ultrasonic cleaning machine;
(9), the water system miillpore filter of 0.45 μ m;
(10), the argon gas of purity 〉=99.99%;
2) configuration reagent and standard solution:
(1), leaching liquor: the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid;
(2), mobile phase: the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid, before using through 0.45 μ m membrane filtration and ultrasonic degas;
All reagent is all that analysis is pure or top grade is pure, and ultrapure water is all used in whole experiment; Glass apparatus uses front through 15% nitric acid dousing 24h;
(3), the standard solution of trivalent aluminium:
Trivalent aluminium standard solution: the storing solution that 100 μ g/mL trivalent aluminium standard solution is diluted to 1.00 μ g/mL trivalent aluminium, putting 4 ℃ of refrigerators deposits standby, trivalent aluminium storing solution by 1.00 μ g/mL is diluted to the trivalent aluminium standard solution of 50.0ng/mL, 100.0ng/mL, 250.0ng/mL, 500.0ng/mL, 1000.0ng/mL, matching while using through mobile phase;
3) step of sample preparation:
Dry sample 0.400g～the 0.800g that takes through pulverizing 40 mesh sieves is placed in 50mL tool plug scale test tube, adding extract 20mL mixes, or bright sample smashs homogenate to pieces and takes 2.000g～4.000g and be placed in 50mL tool plug scale test tube, adds extract 20mL and mixes, to 70 ℃ of water bath with thermostatic control shaking table 1h, after the abundant lixiviate of sample, take out coolingly, the centrifugal 15min of 4000r/min, take out supernatant with the water system filtering with microporous membrane of 0.45 micron, move in sample injection bottle, upper machine is measured the value of trivalent aluminium;
4) experiment instrument condition used:
(1), high-efficient liquid phase chromatogram condition HPLC: mobile phase is the mixed liquor of 0.0040mol/L lithium hydroxide, 0.0060mol/L pyridine-2.6-dicarboxylic acid, 0.090mol/L glacial acetic acid, flow velocity 1mL/min; Sampling volume 50～100 μ L, auto injection;
(2), Inductively coupled plasma mass spectrometry condition ICP-MS: radio-frequency power 1150～1600W, plasma flow speed 15～20L/min, assisted gas flow velocity 1.2～1.5L/min; Sampling time 10min; Measure mass number
27Al;
5) sample detection and result are calculated:
(1), qualitative: as to arrange by above-mentioned condition after start, after stable, first do typical curve, then measure the sample measuring liquid for the treatment of of handling well; Adopt full-automatic injector sample introduction 50～100 μ L to measure under above-mentioned high performance liquid chromatography and Inductively coupled plasma mass spectrometry condition, high performance liquid chromatograph separates, Inductively coupled plasma mass spectrometry pair
27Al detects; The trivalent aluminium retention time is about 3.172min under above-mentioned instrument condition;
(2), quantitative: the chromatographic peak retention time for the treatment of trivalent aluminium in sample measuring liquid is compared variation range and namely think this material to be determined within ± 10% with standard solution;
Result is calculated and statement:
With the external standard method in data processing software, determine trivalent aluminium retention time and degree of separation pulse strength, take concentration as horizontal ordinate, the pulse strength integration is ordinate, the drawing standard working curve,, then with sample liquid peak analyzing and processing, can obtain treating the concentration of the trivalent aluminium in sample measuring liquid, calculate the content of trivalent aluminium in derived sample by following formula (1):
X=C×V/m×1000...............(1)
In formula:
The content of trivalent aluminium in X-sample, mg/kg;
The concentration of trivalent aluminium in C-liquid to be measured, ng/ml;
M-sample weighting amount, g;
V-mensuration total liquid volume, mL.
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| 《润肤霜类化妆品中金属元素的测定及砷形态初探》;林立 等;《环境化学》;20100131;第29卷(第1期);149-151 * |
| 《环境与生物体系中铝形态分析技术的新进展》;杨小弟 等;《分析化学》;20030930;第31卷(第9期);1131-1138 * |
| 《电感耦合等离子体质谱、中子活化分析及其它谱学方法测定环境、生物样品中铝形态和含量研究进展》;林海 等;《分析科学学报》;20041231;第20卷(第6期);652-656 * |
| 杨小弟 等.《环境与生物体系中铝形态分析技术的新进展》.《分析化学》.2003,第31卷(第9期), |
| 林海 等.《电感耦合等离子体质谱、中子活化分析及其它谱学方法测定环境、生物样品中铝形态和含量研究进展》.《分析科学学报》.2004,第20卷(第6期), |
| 林立 等.《润肤霜类化妆品中金属元素的测定及砷形态初探》.《环境化学》.2010,第29卷(第1期), |
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