Method for detecting divalent cadmium ion in aquatic product by using HPLC-ICP-MS coupling technique
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A technology of HPLC-ICP-MS and combined technology, applied in the field of aquatic product detection, to achieve the effect of accurate scientific quality and safety, reasonable selection of experimental conditions, and good separation
Active Publication Date: 2012-07-18
QINGDAO DONGWEI FOOD CO LTD
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At present, there is no method standard for the determination of divalent cadmium ions in aquatic products in the international ISO and CAC standards
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Embodiment 1
[0050] Embodiment 1: the mensuration of divalent cadmium ion i.e. Cd(II) in scallop:
[0051] 1. Instruments and equipment used in this embodiment: HPLC-ICP-MS combined system:
[0052] (1), HPLC (Perkin-Elmer, USA, model Series 200) part: use SERIES200 high-pressure liquid phase pump, equipped with automatic sampler, equipped with guard column CG5A 4 × 50mm and CS5A 4 × 250mm cation of the same material filler exchange column;
[0053] (2), ICP-MS (Perkin-Elmer, USA, model ELAN DRC II) part: equipped with dynamic reaction cell, automatic sample injection system, radio frequency generator, plasma system, Chromera speciation analysis automatic processing interface, ion lens System, quadrupole, vacuum system, detector, gas path control system;
[0054] (3), cooling circulating water (US POLYSCIENCE company, model SHA-C);
[0055] (4), Vortex mixer (IKA MS 3 basic);
[0056] (5), pure water system (Millipore, USA, Milli-Q Gradient A10);
[0057] (6), circulating vacuum sand ...
Embodiment 2
[0089] Embodiment 2: to the mensuration of Cd (II) in laver:
[0090] Weigh 1.000 g of the crushed and dried seaweed sample and place it in a 50 mL plastic graduated centrifuge tube with stopper, add 40 mL of water and mix well. Ultrasonic extraction for 40min, centrifugation at 8000r / min at 4°C for 10min, the supernatant was taken out and filtered with a 0.22 micron water-based microporous membrane, and the value of Cd(II) in the extract was measured on a computer. Other conditions are the same as those of scallops and oysters.
[0091] The standard recovery rate test of the samples in laver showed that the standard recovery rate was 91.2%, and the relative standard deviation was less than 5%, which met the analysis requirements. The determination results of divalent cadmium ions in laver are shown in Table 2.
[0092] Table 2, the assay result of laver spiked recovery (on a dry basis)
[0093]
[0094] In order to ensure the accuracy and reliability of the experimental ...
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Abstract
A method for detecting a divalent cadmium ion in an aquatic product by using an HPLC-ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometer) coupling technique belongs to the technical field of detection of aquatic products. The method comprises the following steps: 1), selecting instruments and equipment as well as an HPLC-ICP-MS coupling system; 2), configuring reagents and a standard solution; 3), processing a sample; 4), creating conditions for the experiment instruments; and 5), detecting the sample and calculating the results. According to the method, the cadmium in the aquatic product is extracted by neutral water in an ultrasonic way and the state of the cadmium is not changed, so that the cadmium in a free ion state and the cadmium subjected to complexation with organic matters such as protein both exist in the extract solution. In the adopted mobile phase, oxalate exerts a strong complexation effect on the cadmium ions but does not adsorb and elute stable cadmium complex in the extract solution, so that the cadmium ions and the cadmium complex in the sample can be guaranteed to be better separated. The method for detecting the divalent cadmium ion in the aquatic product by using the HPLC-ICP-MS coupling technique fills a blank in national standard that only the cadmium detection method is provided but no method for detecting the state of cadmium element is provided, therefore, the quality safety of the aquatic product and products of the aquatic product can be accurately and scientifically evaluated, meanwhile, the method is of great significance for formulating a new standard on the limit of harmful elements in the aquatic product.
Description
Technical field: [0001] The invention belongs to the technical field of aquatic product detection, and in particular relates to a method for measuring divalent cadmium ions in aquatic products by using high performance liquid chromatography-inductively coupled plasma mass spectrometer (HPLC-ICP-MS) combined technology. Background technique: [0002] Cadmium is not an essential trace element for the human body. There is almost no cadmium in the body of newborn babies, and all cadmium in the human body enters the human body through the external environment (such as drinking water, food, and cigarettes) after birth. Studies have shown that cadmium poisoning can cause renal tubular reabsorption disorder, low molecular weight protein and calcium are lost in urine, and in the long run it is easy to form osteomalacia, joint pain, fracture and kidney bone deformation. Long-term intake of excessive cadmium will affect the performance of other beneficial elements in the body, causing...
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