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建立了微生物降解体系中反-4-甲基-环己烷酸(4MCCA)的气相色谱-质谱测定方法。分别采用孔径为0.45和0.22μm滤膜对微生物降解体系中的4MCCA样品进行减压过滤,去除菌体;用0.1 mol/L H2SO4调节滤液至pH 2～3;二氯甲烷萃取定容。利用气相色谱-质谱的选择离子模式检测,外标法定量。本方法的线性范围为0.10～100 mg/L,相关系数为0.9994,检出限和定量限分别为0.10 ng和0.34 ng,日内和日间精密度分别为2.7%～6.6%和1.5%～11.3%。采用本方法测定了150 mg/L 4MCCA在微生物降解体系中的降解情况,24,48和96 h时4MCCA的降解率分别为24.7%,51.8%和55.0%。
A gas chromatography-mass spectrometry method was developed for the determination of trans-4-methyl-cyclohexane acid (4MCCA) in microbial degradation system. The 4MCCA samples in the biodegradation system were respectively filtered under reduced pressure to remove the cells by using 0.45 and 0.22 μm filters. The filtrate was adjusted to pH 2-3 with 0.1 mol / L H2SO4 and extracted with dichloromethane. Selected by gas chromatography - mass spectrometry ion mode detection, external standard quantitative. The linear range of this method was 0.10-100 mg / L with a correlation coefficient of 0.9994. The limits of detection and quantification were 0.10 ng and 0.34 ng, respectively. The intra- and inter-day precision was 2.7% -6.6% and 1.5% -11.3, respectively %. Degradation of 150 mg / L 4 MCCA in the biodegradation system was determined by this method. The degradation rates of 4MCCA at 24, 48 and 96 h were 24.7%, 51.8% and 55.0%, respectively.