摘要
建立了蔬菜中64种农药残留固相萃取-全二维气相色谱-飞行时间质谱(GC×GC-TOF-MS)的测定方法。用乙腈提取样品,NH2-SPE固相萃取柱净化,甲醇-二氯甲烷溶液(5:95,V/V)洗脱,氮气吹扫浓缩,丙酮定容,全二维气相色谱(HP-5MS柱和DB17ht柱)-飞行时间质谱检测,基质曲线外标法定量。本方法的检出限(S/N=3)和定量限(S/N=10)范围分别为0.010～6.032μg/kg和0.035～20.107μg/kg。64种农药在油菜薹、黄瓜、茄子、四季豆和辣椒中的回收率范围为68.3%～117.8%,相对标准偏差为0.6%～9.1%。采用本方法检测市场中样品,发现2例样品中含乙酰甲胺磷和氯氰菊酯残留,测定值分别为0.036和0.107mg/kg。
A solid phase extraction-comprehensive two-dimensional gas chromatography coupled with time-offlight mass Spectrometric（GC × GC-TOF-MS） method for analysis of 64 pesticides in vegetables was developed and validated.After extracting with acetonitrile,cleaning-up with NH2-SPE cartridge and concentrating with nitrogen,the pesticide residues were redissolved in the acetone and analyzed by GC × GC-TOF-MS coupled with HP-5MS and column DB-17 column.Sample matrix-matched calibration was used to determine the residue contents by external standard.The method was validated by the real samples,such as Brassica campestris,cucumber,eggplant,kidney bean and capsicum.The limits of detection（S/N = 3） and the limits of quantification（S/N = 10） were from 0.010 to 6.032 μg/kg and from 0.035 to 20.107 μg/kg,respectively.The overall recoveries ranged from 68.3% to 117.8% with the relative standard deviations（RSD） of 0.6%-9.1%.Two positive samples,polluted by acephate and cypermethrin with a residual concentration of 0.036 and 0.107 mg/kg,were screened by the developed method as detecting markets samples.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2011年第1期72-76,共5页
Chinese Journal of Analytical Chemistry
基金
国家科技支撑计划(No.2009BADB9B03-Z09)
武汉市青年科技晨光计划(No.200950431224)资助
关键词
全二维气相色谱-飞行时间质谱
农药残留
蔬菜
Comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry
Multiple pesticide residues
Vegetable
