CAJ | 학술논문

采用四乙基硼酸钠( NaBEt4)为衍生剂,建立简单、高效的生物样品有机锡气相质谱( GC-MS)分析方法。结果表明,冷冻干燥生物样品粉末0.1 g经15 mL 0.035 mol/L盐酸甲醇振荡提取1 h,定量提取液加入乙酸盐缓冲溶液(pH 4.8)调节溶液酸度,用含内标物正己烷2 mL和0.5 mL 2%(m/V)NaBEt4水溶液衍生萃取30 min后,GC-MS同时测定一丁基锡( MBT)、二丁基锡(DBT)、三丁基锡(TBT)。在0.5~50μg/L范围内,线性良好,3种有机锡加标回收率均在80%以上。此方法能快速简单对复杂生物样品中的有机锡进行分析,其检出限约为0.01μg/L,3个平行样测量值标准偏差都在10%以内。
채용사을기붕산납( NaBEt4)위연생제,건립간단、고효적생물양품유궤석기상질보( GC-MS)분석방법。결과표명,냉동간조생물양품분말0.1 g경15 mL 0.035 mol/L염산갑순진탕제취1 h,정량제취액가입을산염완충용액(pH 4.8)조절용액산도,용함내표물정기완2 mL화0.5 mL 2%(m/V)NaBEt4수용액연생췌취30 min후,GC-MS동시측정일정기석( MBT)、이정기석(DBT)、삼정기석(TBT)。재0.5~50μg/L범위내,선성량호,3충유궤석가표회수솔균재80%이상。차방법능쾌속간단대복잡생물양품중적유궤석진행분석,기검출한약위0.01μg/L,3개평행양측량치표준편차도재10%이내。
A simple and efficient method for the determination of organotin compounds ( OTCs) in biota by GC-MS coupling with sodium tetraethylborate ( NaBEt4 ) derivatization was established. The results showed that recoveries for each OTCs spiked in blank freeze-dryed biological samples ( 0 . 1 g ) following extraction (15 mL 0. 035 mol/L methanolic HCl solution for 1 h ) and derivatization (2 mL contained internal standard n-hexane and 0. 5 mL of 2% (m/V) NaBEt4 solution for 30 min) were above 80%. The method is fast and easy to operate for the determination of OTCs in complex biological samples. The minimum limit of detection was about 0. 01 μg/L, and relative standard deviation values were within 10% for three parallel samples.