Study On Analytical Method Of Tributyltin And Triphenyltin In Food

Organotin is endocrine disruptor. Its use will cause environmental pollution worse and will seriously harm human health by the food chain transmission. Therefore, it has important significance to detect the organotin compounds in food. At present, most of the analysis are more concentrated on environmental samples. The research reports on organotin compounds in food are relatively few. In the article, we systematically research the determination methods of organotin in food. The research results are as follows:1. GC-FPD was applied to detect tributyltin(TBT) and triphenyltin(TPhT) in wine. The wine was extracted by liquid liquid extraction and the chromatographic separation conditions and derivation conditions of tributyltin and triphenyltin were explored. In the range of 0.1～10mg/L, the derivation peak area and organotin concentration assumed a good linear relationship, with correlation coefficients of 0.9990,0.9995 and limits of detection of 0.038mg/L,0.049mg/L, respectively. In the three spiked level, the average recoveries of tributyltin and triphenyltin are in the range of 89.8%～100.9% with relative standard derivation of 4.2%～9.0%. This method can be effectively used in the determination of organotin compounds in wine.2. GC-FPD was applied to detect tributyltin and triphenyltin in rice. The rice sample was extracted with CH2Cl2 by ultrasonic extraction and extracts were cleaned up with column chromatography. In the range of 0.1～10mg/L, the derivation peak area and organotin concentration assumed a good linear relationship, with correlation coefficients of 0.9990,0.9995 and limits of detection of 0.038mg/L,0.049mg/L, respectively. In the three spiked level, the average recoveries of tributyltin and triphenyltin are in the range of 96.4%～109.4% with relative standard derivation of 4.1%～8.5%. This method can be effectively used in the determination of organotin compounds in rice.3. A new method was established for detecting tributyltin and triphenyltin in fish by GC-FPD. The fish sample was extracted with hexane-acetone (1/1,V/V) by microwave-assisted extraction and the orthogonal experiment design was used to optimize extraction conditions.The extract was derivatived with NaBEt4 and cleaned up by dispersive solid phase extraction and the conditions of derivation, purifying were optimized. In the range of 0.1～10mg/L, the derivation peak area and organotin concentration assumed a good linear relationship, with correlation coefficients of 0.9991,0.9996 and limits of detection of 0.038 mg/L,0.049 mg/L, respectively. In the three spiked level,the average recoveries of tributyltin and triphenyltin are in the range of 96.5%～116.2% with relative standard derivation of 4.0%～9.3%. This method was used in the determination of organotin compounds in fish with good results.4. A method was developed for the determination of tributyltin and triphenyltin in laver by GC-FPD.The laver was extracted with ethyl acetate-hexane (4/1,V/V) by ultrasonic extraction and the extraction conditions of TBT,TPhT was optimized by the response surface analysis. The extract was derivatived with NaBEt4, cleaned up by dispersive solid phase extraction and the quantity of activated -carbon on purifying efficiency of TBT and TPhT was examined. In the range of 0.1～10 mg/L, the derivation peak area and organotin concentration assumed a good linear relationship, with correlation coefficients of 0.9989,0.9996 and limits of detection of 0.038 mg/L,0.049mg/L, respectively. In the three spiked level, the average recoveries of tributyltin and triphenyltin are in the range of 80.3%～106.9% with relative standard derivation of 5.1%～8.7%. This proposed method was applied to determine TBT, TPhT in laver with good results.5. HPLC-ICP-MS was used to detect tributyltin and triphenyltin in laver. The laver sample was extracted with ethyl acetate-hexane (1/1,V/V) by ultrasonic extraction and cleaned up by dispersive solid phase extraction. After that, The chromatographic separation condition of TBT and TPhT was optimized. In the range of 4～20μg/L, the derivation peak area and organotin concentration assumed a good linear relationship, with correlation coefficients of 0.9990,0.9991 and limits of detection of 0.37μg/L,0.49μg/L, respectively. In the three spiked level, the average recoveries of tributyltin and triphenyltin are in the range of 96.8%～112.6% with relative standard derivation of 3.2%～9.3%. This method is rapid, accurate, can be used to detect TBT and TPhT in laver. The proposed method was successfully applied to the determination of TBT and TPhT in laver.