- DETERMINATION OF 3,3',4,4'-TETRACHLOROAZOBENZENE IN WATER BY ISOTOPE DILUTION GAS CHROMATOGRAPHY/HIGH RESOLUTION MASS SPECTROMETRY
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A methodology, based on gas chromatography/high resolution mass spectrometry selected ion monitoring (GC/HRMS SIM) has been developed for the determination of 3,3',4,4'-tetrachloro-azobenzene (TCAB), a potential carcinogen, in water. As internal standard we prepared labelled TCAB, from labelled benzene. TCAB was extracted from water by hexane followed by a cleanup column chromatography over basic alumina. Recoveries of TCAB range from 80.0-88.3 percent. The detection limit of TCAB is about 50 fg of TCAB or 5 ppq in 1,000 mL of water.
- Schneider, Serge,Hashimoto, Shunji,Yamamoto, Takashi,Morita, Masatoshi
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- Stable isotope labeled zearalenone and synthesis method thereof
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The invention discloses stable isotope labeled zearalenone and a synthesis method thereof. The method comprises the following steps: by taking stable isotope C-labeled benzene-C6 as a starting raw material, carrying out nitration reaction, nitro reduction reaction, benzene ring bromination reaction, amino elimination reaction, methoxylation reaction, aldehyde group oxidation reaction and demethylation reaction to obtain stable isotope C-labeled 2, 4, 6-trihydroxybenzoic acid-benzene ring-C6, and then carrying out lactonization reaction of hydroxyl and carboxyl, methyl reaction in Mitsunobu reaction, Stille reaction, reaction of oxidizing hydroxyl into aldehyde group, esterification reaction of carboxylic acid and alcohol, reaction of oxidizing hydroxyl into ketone carbonyl group, olefin metathesis reaction, olefin selective reduction reaction and the like. According to the invention, stable isotope labeled zearalenone-benzene ring-6 is obtained through a total synthesis method for the first time, raw materials are cheap and easy to obtain, reaction products in all steps are easy to separate and purify, the yield is high, and the chemical purity and the stable isotope abundance both reach 98% or above.
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Paragraph 0042-0043;0082
(2021/06/22)
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- A stable isotope labeling prohibited pigment synthesis method
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The invention relates to a synthesizing method for a prohibited pigment labeled by a stable isotope. According to the synthesizing method, bromobenzene labeled by a stable isotope D or 13C is aminated and sulfonated to synthesize an intermediate sodium sulfanilate labeled by the stable isotope D or 13C, or the bromobenzene is taken as the raw materials and then aminated and sulfonated with an ammoniation reagent labeled by a stable isotope 15 N to synthesize the intermediate sodium sulfanilate labeled by the stable isotope 15N, and then diazotizing and coupling are performed to synthesize the prohibited pigment labeled by the stable isotope D or 15N or 13C. Compared with the prior art, the synthesizing method has the advantages that the process route is simple, the prohibited pigment labeled by the stable isotope is easy to synthesize, the product is easy to separate and purify, the chemical purity of the product is more than 99.0 percent, the isotope abundance is more than 98.0 percent, the requirements of trace detection in the field of food safety can be fully met, and the good economical efficiency and use value are achieved.
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Paragraph 0055; 0056; 0062; 0063; 0112; 0119; 0126; 0133
(2017/10/13)
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