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A determination method and technology of inorganic arsenic, which are applied in measurement devices, instruments, scientific instruments, etc., to achieve the effects of reasonable selection, complete extraction, and accurate and reliable detection data.
Inactive Publication Date: 2008-09-10
YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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In 2006, the controversy over the limit indicators in the current national health standard GB19643-2005 "Hygienic Standard for Algae Products" in seaweed food and the national standard GB/T5009.11-2003 "(Detection method of total arsenic and inor
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Embodiment 1
[0065] Embodiment 1: the mensuration of inorganic arsenic in sea-tangle:
[0066] 1. Selected instruments and equipment: HPLC-HGAFS combined system:
[0067] (1), HPLC part, using LC-10ATVP high-pressure liquid phase pump; equipped with 7725i six-way sampling valve (Rheodyne, Cotati, CA, USA) with 100 μ L quantitative loop; equipped with the same material packing guard column (25mm × 2.3mm i.d, 12-20 μm) PRP-X100 (250mm×4.1mm i.d, 10 μm) anion exchange column (Hamilton, Reno, NV);
[0069] (3), water bath constant temperature oscillator (Shanghai Hexin Instrument Co., Ltd., model SHA-C);
[0070] (4), sand core filter (sand core filter device, model SH / T0093);
[0071] (5), circulating vacuum pump (circulating vacuum pump, model SHZ-D);
[0072] (6), ...
Embodiment 2
[0116] Embodiment 2: the mensuration of inorganic arsenic in prawn:
[0117] Weigh 3.0000 g of the sample (need to be crushed and homogenized) into a 50 mL graduated test tube with stopper, add 20 mL of 10% hydrochloric acid solution, and mix well. Put it in a constant temperature shaker in a water bath at 70°C for 1 hour to fully extract the sample. Take it out, cool it down to 25ml, and filter it with absorbent cotton. Take 2mL supernatant to a 10ml tube, add 1.6mL HO 2 O, 0.4mLH 2 o 2 After mixing, put it in a 70°C water bath for 20 minutes, take it out and filter it with a 0.45 micron water-based microporous membrane, and measure the inorganic arsenic value on the machine. Other conditions are the same as that of kelp, and the determination results of the recovery rate of the prawn spiked (see Table 4).
[0118] Table 4, the assay result of prawn spiked recovery rate (in fresh basis)
[0119] Determining elements
Background measurement
ng / mL
...
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Abstract
The invention relates to a determination method for inorganic arsenic in aquatic products. After being extracted by hydrochloric acid solution, the inorganic arsenic (1plus1) in the aquatic products passes through an anion-exchange column, and arsenite As (III), dimethyl arsenic compound DMA, methyl arsenic compound MMA and arsenate As (V) are eluted sequentially by mobile phase; owing to different adsorption capacities of the anion-exchange column on the arsenate As (V), the arsenite As (III), the methyl arsenic compound MMA, the dimethyl arsenic compound DMA and arsenic sugar AsS, the eluted solution is hydrogenated by borohydride potassium reducing agent and hydrochloride, and hydride is generated, enters an atomizer, and is subject to analytic determination by being combined with atomic fluorescence. The experimental condition is reasonably selected, and the detecting data is accurate and reliable and can not be influenced by extraction time and temperature. The determination method of inorganic arsenic in aquatic products of the invention not only can detect the inorganic arsenic iAs accurately, but also can determine the methyl arsenic compound MMA and the dimethyl arsenic compound DMA of the organic arsenic, and can be used for the morphometry of the arsenic in the aquatic products.
Description
Technical field: [0001] The invention belongs to the detection technology of aquatic products, and relates to a method for measuring inorganic arsenic in aquatic products by using high-performance liquid chromatography-hydride generation atomic fluorescence spectrometry (HPLC-HGAFS) form analysis technology. Background technique: [0002] Currently, one of the frontiers of elemental analytical chemistry is the qualitative and quantitative determination of different forms of elements, not just the total amount of elements, mainly because different forms of the same element may have completely different chemical and toxicological properties , arsenic is a typical element. The main forms of arsenic are: arsenate As (V), arsenite As (III), monomethyl arsenic compound (MMA), dimethyl arsenic compound (DMA), trimethyl arsenic oxide (TMAO ), arsenobetaine (AsB), arsenocholine (AsC) and arsenosugar (AsS), among which inorganic arsenic (iAs) [including As(V), As(III)] is highly toxi...
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IPC IPC(8): G01N30/88
Inventor 尚德荣翟毓秀宁劲松王联珠冷凯良
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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