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建立了葡萄酒中一丁基锡、二丁基锡和三丁基锡检测的两种分析方法,分别采用液液萃取法(LLE)和固相微萃取法(SPME),以四乙基硼化钠为衍生试剂,气相色谱-串联质谱(GC-MS/MS)检测,内标法定量。对两种方法的萃取条件(萃取时间、温度等)、衍生条件(pH、衍生试剂用量等)和GC-MS/MS条件进行了选择和优化。考察和对比了两种方法的灵敏度和准确度。结果表明,LLE和SPM E法的检出限分别为0.5μg/kg(以Sn计,下同)和0.01μg/kg,针对干红、干白和桃红3种葡萄酒基质,在4个添加水平下的回收率范围分别为70.7%~103.3%和61.7%~114.1%,RSD范围分别为2.2%~8.4%和6.6%~16.0%。LLE法稳定性好,方法准确可靠;SPM E法虽精密度稍差,但具有极高的灵敏度,而且操作简便,不需消耗有机溶剂。两种方法联合使用具有较宽的检测范围,适用于葡萄酒中丁基锡化合物的检测。
Two analytical methods for the determination of monobutyltin, dibutyltin and tributyltin in wine were established. Liquid-liquid extraction (LLE) and solid-phase microextraction (SPME) were used respectively. Tetraethyl sodium boride was used as the derivatization reagent, Chromatography - tandem mass spectrometry (GC-MS / MS) detection, internal standard method. The extraction conditions (extraction time, temperature, etc.), derivatization conditions (pH, amount of derivatization reagent, etc.) and GC-MS / MS conditions were optimized and optimized for both methods. The sensitivity and accuracy of the two methods were examined and compared. The results showed that the detection limits of LLE and SPM E were 0.5μg / kg (in terms of Sn, the same below) and 0.01μg / kg, respectively. For the three wine bases of dry red, dry white and pink, The recoveries ranged from 70.7% to 103.3% and from 61.7% to 114.1%, respectively, with RSD ranges of 2.2% -8.4% and 6.6% -16.0%, respectively. LLE method has good stability and the method is accurate and reliable. Although the SPM E method is less precise, it has high sensitivity and is easy to operate without consuming organic solvents. The combination of the two methods has a wide range of detection, suitable for the detection of butyltin compounds in wine.