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目的建立气相色谱-三重四极杆串联质谱法,测定蟑螂药及其中毒样品中乙酰甲胺磷和残杀威的分析方法,为蟑螂药中毒的快速诊断及治疗提供准确的实验室依据。方法本方法用丙酮或乙睛提取,CARB/NH_2固相萃取柱净化,旋转蒸发仪至近干,氮气吹干,丙酮准确定容后,用TR-PESTICIDEⅡ(30 m×0.25 mm,0.25μm)毛细管色谱柱分离,气相色谱-三重四级杆串联质谱法测定,外标法定量。结果用本方法测定,乙酰甲胺磷和残杀威色谱峰得到很好分离,乙酰甲胺磷在0.05μg/ml~1.50μg/ml、残杀威在0.01μg/ml~0.30μg/ml时均呈良好的线性关系,相关系数可达0.999。乙酰甲胺磷、残杀威的最低检出限分别为0.06 mg/kg、0.012 mg/kg。相对标准偏差为3.2%~9.3%,回收率为92.2%~108.2%。结论该方法样品用量少、简便快速、灵敏度高、结果准确可靠,能够满足中毒样品分析的实验要求。
OBJECTIVE To establish a method for the determination of acephate and propoxur in cockroach and its poisoned samples by gas chromatography-triple quadrupole tandem mass spectrometry, to provide an accurate laboratory basis for the rapid diagnosis and treatment of cockroach poisoning. Methods The samples were extracted with acetone or acetonitrile, cleaned up on a CARB / NH 2 solid phase extraction column, dried to near dryness with a rotary evaporator, dried under nitrogen, Column separation, gas chromatography - triple quadrupole mass spectrometry, external standard method. Results The results of this method showed that the acephate and propoxuril peaks were well separated. Acephate ranged from 0.05μg / ml to 1.50μg / ml, and propoxurone from 0.01μg / ml to 0.30μg / ml Good linearity with a correlation coefficient of 0.999. The detection limits of acephate and propoxur were 0.06 mg / kg and 0.012 mg / kg, respectively. The relative standard deviations were 3.2% ~ 9.3% and the recoveries were 92.2% ~ 108.2%. Conclusions This method has the advantages of less amount of sample, simple and quick method, high sensitivity and accurate and reliable results, which can meet the experimental requirements of the analysis of poisoned samples.