Detection method of dibutyl phthalate in traditional Chinese medicinal materials
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A dibutyl phthalate and detection method technology, applied in the field of analysis and testing, can solve problems such as unreported research on dibutyl phthalate, achieve good precision and reproducibility, and improve accuracy Effect
Inactive Publication Date: 2012-07-25
JILIN INST OF CHEM TECH
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Problems solved by technology
[0006] At present, there are many detection methods and relevant researches on phthalates in food packaging bags, but there is no report on dibutyl phthalates in Chinese herbal medicines
Method used
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Embodiment 1
[0033] 1 Preparation of sample solution
[0034] Weigh 5.00g (40 mesh) of crushed corn silk stigma and style, put it into a 100mL round bottom flask, add dichloromethane to soak for 0.5h, oscillate ultrasonically for 15-35min, then reflux at 60°C for 1h, extract twice , combine the extracts, concentrate to 1 / 4 to 1 / 6 of the original volume, add water to disperse the extraction, dehydrate the extract with anhydrous sodium sulfate, filter, and concentrate. Draw 1mL of the sample extract and pass it through a 500mg / 3mLODS solid-phase extraction column activated with dichloromethane in advance for concentration and enrichment. The eluate was collected by blowpipe, concentrated to 1 mL by nitrogen blowing, passed through a 0.45 μm disposable syringe micro-membrane filter, and directly injected by gas chromatography for analysis.
[0035] 2 Chromatographic conditions
[0036] The inlet temperature was 280°C, and the FID temperature was 300°C. Column temperature: using temperature...
Embodiment 2
[0040] 1 Preparation of sample solution
[0041]Weigh 5.00 g (40 mesh) of both tips after crushing, put it into a 100 mL round bottom flask, add dichloromethane to soak for 0.5 h, oscillate ultrasonically for 15-35 min, then reflux at 60°C for 1 h, extract twice, and combine the extracts , concentrated to 1 / 4 to 1 / 6 of the original volume, added water to disperse and extract, the extract was dehydrated with anhydrous sodium sulfate, filtered, and concentrated. Draw 1mL of the sample extract and pass it through a 500mg / 3mLODS solid-phase extraction column activated with dichloromethane in advance for concentration and enrichment. The eluate was collected by blowpipe, concentrated to 1 mL by nitrogen blowing, passed through a 0.45 μm disposable syringe micro-membrane filter, and directly injected by gas chromatography for analysis.
[0042] 2 Chromatographic conditions
[0043] The inlet temperature was 280°C, and the FID temperature was 300°C. Column temperature: using tempe...
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Abstract
The invention discloses a detection method of environmental hormone dibutyl phthalate (DBP) in traditional Chinese medicinal materials, which belongs to the technical field of analysis and detection, and comprises the following steps of carrying out ultrasonic-assisted extraction on the traditional Chinese medicinal materials, and carrying out secondary purification, namely a purification method of removing water-soluble impurities by dichloromethane-water phase liquid-liquid partition, and removing fat-soluble impurities by an ODS (octadecyl silane)-C18 solid phase column is adopted; and the advantages of high GC-FID (gas chromatography-flame ionization detector) sensitivity, good separation effect and accuracy in quantification are utilized, so that the degree of accuracy, the degree of precision and the reproducibility can be ensured. Potential long-term harms can be formed when people take foods or the traditional Chinese medicinal materials containing the environmental hormone dibutyl phthalate for a long time; and therefore, conditions of higher requirements on cultivation, transportation and storage of the traditional Chinese medicinal materials need to be proposed, and strengthening monitoring and early warning on DBP has certain practical applicability, and the method has significance. The detection method can accurately detect the DBP content in the traditional Chinese medicinal materials, and is low in cost, and is simple, convenient and fast.
Description
technical field [0001] The invention relates to a gas chromatography detection method for dibutyl phthalate in Chinese medicinal materials, belonging to the field of analysis and testing. Background technique [0002] Phthalates (PAEs) are the main body of plasticizers. It is widely used in daily life because of increasing the plasticity and flexibility of products. In the past, PAEs were considered to be low in toxicity, but in recent years, the results of animal toxicity tests have shown that PAEs have reproductive toxicity, embryotoxicity, and genotoxicity, especially the abnormal human reproductive function. Due to the long residual period of PAEs in the environment and the enrichment effect of organisms on them, my country has included dimethyl phthalate (DMP), diethyl phthalate (DEP) and phthalate in the PAEs family. Di-n-octyl formate (DNOP) is identified as an environmental priority control pollutant. "National Drinking Water Standard" (GB5749-2006) requires DEHP&l...
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