建立了五氟苯甲酰氯衍生-气相色谱-质谱法测定地表水中一甲基肼的方法.取200ml水样,调节后的pH为10,加入20ml衍生剂,在室温下剧烈振荡衍生1h,40ml二氯甲烷萃取10min,浓缩至1.0ml后用气相色谱-质谱联用分析.方法在5～500μg/L浓度范围内线性良好,相关系数大于0.996,方法检出限为2.67μg/L；加标水样的相时标准偏差为9.54％和8.38％;加标水样回收率为79.08％～102.96％.%The method was established to determine the methylhydrazine by pentafluorobenzoyl chloride derivatization in surface water coupled with gas chromatography - mass spectrometry. The volume of water sample was 200ml,the adjusted value of pH was 10, the amount of derivative reagents was 20ml, the lime of derivatizalion was lh, the way of derivatization was shaking violently. After derivatization ending, the derivatization solution was extracted l0min by 40ml dichloromethane. After extraction solution was concentrated to 1 ml, gas chromatography - mass spectrometry was used for quantitative and confirmatory analysis of the derivative product. The method linearity range was 5 - 500ng/L. The correlation coefficient was not less than 0. 996. The detect limit of the method was 2. 67ug/L. The RSD of (he spiked samples were 9. 54% and 8. 38% , respectively. The recovery of the spiked samples was 79. 08% ~ 102. 96% .
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