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建立了测定大豆、糙米、黄瓜、甜菜等6种植物源性农产品中噁霉灵残留的气相色谱-火焰光度法(GC-FPD)、气相色谱-氮磷检测法(GC-NPD)和液相色谱-串联质谱法(LC-MS/MS)。GC-FPD法采用丙酮-正己烷提取样品,O,O-二甲基硫代磷酰氯衍生,GC-FPD分析,外标法定量;GC-NPD法采用丙酮-正己烷提取样品,十八烷基键合硅胶(C18)净化,GC-NPD分析,外标法定量;LC-MS/MS法,样品采用乙腈提取,石墨化碳黑(GCB)净化,LC-MS/MS分析,基质匹配外标法定量。结果表明,噁霉灵的响应值与其浓度间呈良好的线性关系,3种方法的相关系数均大于0.998。在3个加标浓度下,GC-FPD法中噁霉灵的日间平均回收率为82%~96%,日间相对标准偏差(RSD)为3.4%~12.1%,方法的定量下限为0.25 mg/kg(甜菜为0.05 mg/kg);GC-NPD法的日间平均回收率为81%~103%,日间RSD为4.1%~14.3%,定量下限为0.25 mg/kg(甜菜为0.05 mg/kg);LC-MS/MS法的日间平均回收率为74%~110%,日间RSD为2.5%~10.7%,定量下限为0.05 mg/kg。3种方法均具有良好的准确性和稳定性,可满足噁霉灵残留分析的要求。
Gas chromatography-flame photometry (GC-FPD), gas chromatography-nitrogen and phosphorus detection (GC-NPD) and liquid-phase spectrophotometry (GC-NPD) were established for the determination of hymexazol residues in six kinds of plant-derived agricultural products such as soybean, brown rice, cucumber and sugar beet, Chromatography-tandem mass spectrometry (LC-MS / MS). GC-FPD method using acetone - n-hexane samples, O, O-dimethyl thiophosphoryl chloride derivatization, GC-FPD analysis, external standard quantification; GC-NPD method using acetone - n-hexane samples, octadecane LC-MS / MS method, the sample was extracted with acetonitrile, GCB purification, LC-MS / MS analysis, the matrix match outside Standard method of quantitative. The results showed that the response value of hymexazol and its concentration showed a good linear relationship, the correlation coefficients of the three methods were greater than 0.998. At 3 spiked concentrations, the average daily recoveries of hymexazol by GC-FPD ranged from 82% to 96% with a relative standard deviation (RSD) of 3.4% to 12.1% during daytime. The lower limit of quantitation was 0.25 The average day-to-day recoveries of GC-NPD method ranged from 81% to 103% with daytime RSD from 4.1% to 14.3% with a lower limit of quantitation of 0.25 mg / kg for Beet The average day-to-day recoveries of LC-MS / MS ranged from 74% to 110%. The daytime RSD ranged from 2.5% to 10.7%. The lower limit of quantitation was 0.05 mg / kg. All three methods have good accuracy and stability, which can meet the requirements of hymexazol residue analysis.