A method for detecting the purity of thioorganoarsenic finished products
A detection method and technology for finished arsenic products are applied in the field of detection of the purity of thioorganic arsenic finished products, which can solve the problems of misjudgment of the nature of the sample itself, poor stability of thioorganic arsenic, overestimation of sulfur-containing organic arsenic compounds, etc. Simple and easy to operate, solve the problem of accurate analysis of purity, good controllability and reproducibility
Active Publication Date: 2022-04-22
JIANGHAN UNIVERSITY
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Problems solved by technology
Due to the poor stability of thioorganoarsenic, there is no commercial standard product, and laboratory synthetic samples are often used in scientific research for follow-up experiments. After the existing forms are separated, the percentage of the response value of this form to the total response value of all forms is used for rough estimation
However, the response sensitivity of different arsenic species in the equipment is not exactly the same, therefore, this rough quantification method may underestimate or overestimate the content of sulfur-containing organoarsenic compounds in synthetic samples, which may lead to the inconsistency of the samples themselves in subsequent studies. Misjudgment of nature
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Embodiment 1
[0068] Step 1. Configuration of the actual sample:
[0069] Accurately weigh 5mg DMMTA respectively V Synthetic samples and 5 mg DMDTA V Synthetic samples (Cullen, W.R.; Liu, Q.; Lu, X.; McKnight-Whitford, A.; Peng, H.; Popowich, A.; Yan, X.; Zhang, Q.; Fricke, M.; Sun , H., Methylated and thiolated arsenic species for environmental and health research—A review on synthesis and characterization. Journal of Environmental Sciences, 2016, 49, 7-27.), to DMMTA V Add 1 mL of 2% chloroform / ultrapure water, DMDTA to synthetic samples V Add 1mL of 2% ethanol / ultrapure water to the synthetic sample to help dissolve (chloroform and ethanol are both used as help solvents), vortex appropriately, and place an ultrasonic cleaner to gently sonicate to help dissolve until the powder is completely dissolved, and prepare 5mg / mL DMMTA respectively V Synthetic sample stock solution and 5mg / mL DMDTA V Synthetic sample mother liquor.
[0070] Step 2, use inductively coupled plasma mass spectro...
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The invention belongs to the technical field of detection of thioorganoarsenic finished products, and in particular relates to a detection method for the purity of thioorganoarsenic finished products. Include the following steps: Take DMMTA V Finished products and DMDTA V The finished products are respectively dissolved in water or organic solvents to obtain DMMTA V Finished test solution and DMDTA V The finished test solution is tested by HPLC-ICP-MS, combined with the total arsenic content in the test solution, the content of other arsenic components, and the response value data, the DMMTA is determined according to the binary linear equation V and DMDTA V Response factors x and y in HPLC‑ICP‑MS. The detection method is easy to operate, has good controllability and repeatability, and eliminates the need for recovery and determination of all isolated forms of the compound. The content and purity information of the compound can be obtained at the same time as the form analysis, which solves the problem of the unlabeled compound DMMTA. V and DMDTA V Accurate analysis of the purity of the finished product.
Description
technical field [0001] The invention belongs to the technical field of detection of thioorganoarsenic finished products, and in particular relates to a detection method for the purity of thioorganoarsenic finished products. Background technique [0002] Due to natural or man-made sources, arsenic is widely distributed in various environmental media and is a toxic pollutant that seriously affects human health and has a potential carcinogenic risk. There are many kinds of arsenic metabolites, the sample matrix is complex, and the metabolic intermediates are unstable. Thioorganoarsenic compounds are a new class of arsenic metabolites discovered recently, among which the toxicity of monothiodimethylarsenic acid is comparable to that of the more toxic arsenous acid, and monothiodimethylarsenic acid and dithiodimethylarsenic acid Methyl arsenic acid, two currently discovered and detected thioorganoarsenic compounds, can be transformed into each other. Therefore, it is necessary...
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IPC IPC(8): G01N30/02G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/34G01N30/7233G01N30/8675
Inventor 龙艳敏钟慧芳陈程雷梦瑾凌倩倩蔡勇
Owner JIANGHAN UNIVERSITY