人工晶状体样品用丙酮超声提取使残留的2-氯乙醇(ECH)进入溶液中,所得提取液用气相色谱-质谱法(GC-MS)测定其中ECH的含量。GC分析条件:① 采用ZB-624色谱柱,进样品温度180 ℃,分流比1比1;② 载气为高纯氦气,流量为1.5 mL·min-1;③ 升温程序:初始温度50 ℃,保持1 min;以5 ℃·min-1速率升至100 ℃,保持1 min。MS分析条件:离子源温度230 ℃,接口温度250 ℃,电子能量70 eV。以保留时间和质谱全扫描方式进行定性分析,质量数范围m/z 35~500。以选择离子监测模式定量,质量数m/z 43的条件下用外标法定量。方法的理论塔板数在56 753以上。ECH的线性范围为1.44~22.96 mg·L-1,检出限(3S/N)为0.41 mg·L-1。用标准加入法测得方法的回收率为99.1%,测定值的相对标准偏差(n=5)小于5%。

Ethylene chlorohydrin (ECH) was extracted from the sample with acetone. The extract containing the analyte was then analyzed by GC-MS in hyphenation under the following conditions. GC analytical conditions: ① ZB-624 chromatographic column was used, with a temperature of 180 ℃ at the inlet of sample and effluent splitting ratio of 1 to 1; ② high purity helium was used as carrier gas, with a flow-rate of 1.5 mL·min-1; ③ program of temperature elevation: keeping for 1 min at the initial temperature of 50 ℃, raising to 100 ℃ at a rate of 5 ℃·min-1 and keeping for 1 min at 100 ℃. MS analytical conditions: ① temperature of ionic source: 230 ℃; ② temperature at the interface of GC and MS: 250 ℃; ③ electrical energy: 70 eV. Retention time and full-scanning in the mass range of m/z 35 to 500 were used for qualitative analysis; and external standard method under SIM mode with selected ion of m/z 43 was used for quantification of ECH. The number of theoratical plates of this method was found higher than 56 753. Linearity range found for ECH was between 1.44 to 22.96 mg·L-1 and the detection limit (3S/N) was found to be 0.41 mg·L-1. Recovery was tested by standard addition method, giving value of recovery 99.1%. Value of RSD′s (n=5) was less than 5%.