气相色谱-三重四级杆串联质谱法测定蟑螂药及其中毒样品中的乙酰甲胺磷和残杀威

Determination of acephate and propoxur in cockroach medicine and its poisoning samples with gas chromatography-triple quadrupole mass spectrometry

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 A method for determination of acephate and propoxur in cockroach medicine and its poisoning samples with gas chromatography- triple quadrupole mass spectrometry is established so as to provide accurate laboratory basis for the rapid diagnosis and treatment of cockroach medicine poisoning. Methods The samples were extracted with acetone or acetonitrile,clearied up by CARB / NH_2solid- phase extraction column,dried nearly up rotary evaporator,dried by nitrogen,quantified accurately with acetone,and finally isolated and determined by GC- MS / MS with TR- PESTICIDE Ⅱ（ 30 m × 0. 25 mm,0. 25 μm） capillary chromatographic column. Results The chromatographic peaks of acephate and propoxur were separated well by this method. When the concentrations of acephate and propoxure were within 0. 05 μg / ml- 1. 50 μg / ml and 0. 01 μg / ml-0. 30 μg / ml,a good linear relationship was obtained,their correlation coefficient was 0. 999. The minimum detection limits of acephate and propoxur were 0. 06 mg / kg and 0. 012 mg / kg,with the relative standard deviation among 3. 2%- 3. 2%,and the recovery rate among 92. 2%- 108. 2%. Conclusion The method is simple,rapid,sensitive and accurate,requiring less sample and can meet the requirements of analysis on the poisoning samples.