甲醛、乙醛衍生化条件的探讨

Study on the Derivatization conditions for Formaldehyde and Acetaldehyde

关键词:  甲醛  乙醛  衍生化反应  液相色谱  安全监测

Key words:  formaldehyde  acetaldehude  derivatization reaction  HPLC  safety monitoring

摘要:

目的 建立通过HPLC方法同时控制甲醛量、乙醛量的衍生化条件。方法 甲醛、乙醛与2,4-二硝基苯肼溶液在60 ℃水浴中加热60 min衍生化反应，采用Agilent TC-C₁₈色谱柱(4.6 mm×250 mm，5 μm)，以水-乙腈(45∶55)为流动相，流速1.0 mL·min^-1，检测波长350 nm；柱温为40 ℃；进样量20 μL。结果 甲醛、乙醛衍生化物峰的分离度为7.2，甲醛的线性范围为0.028~9.23 μg·mL^-1(r=0.999 4)，平均回收率(n=9)为102.6%(RSD=0.9%)，定量限为3.7×10^-6 μg、检测限为1.8×10^-6μg；乙醛的线性范围为0.063~20.90 μg·mL^-1(r=0.999 5)，平均回收率(n=9)为102.0%(RSD=1.2%)，定量限为1.1×10^-4 μg、检测限为5.5×10^-5 μg。结论 本法准确、灵敏，为甲醛、乙醛的安全监测提供检测依据。

Abstract:

OBJECTIVE To establish the derivatization conditions for controlling the contents of formaldehyde and acetaldehyde by HPLC method at the same time. METHODS After derivatization of which formaldehyde and acetaldehyde was mixed thoroughly with the reagent solution (2,4-DNPH) and heated at 60 ℃ in a water bath for 60 min, the test was performed on Agilent TC-C₁₈ (250 mm×4.6 mm, 5 μm) column with the mobile phase of water-acetonitrile (45∶55) at a flow rate of 1.0 mL·min^-1. The detection wavelength was set at 350 nm and the column temperature was 40 ℃. The injection volume was 20 μL. RESULTS The resolution of the mixture solution of derivatization was 7.2. The linear ranger of formaldehyde was 0.028~9.23 μg·mL^-1 (r=0.999 4), the average recovery (n=9) was 102.6% (RSD=0.9%), LQDformaldehyde was 3.7×10^-6 μg, LODformaldehyde was 1.8×10^-6μg; The linear ranger of acetaldehyde was 0.063~20.9 μg·mL^-1(r=0.999 5), the average recovery (n=9) was 102.0% (RSD=1.2%), LOQacetaldehyde was 1.1×10^-4 μg, LODacetaldehyde was 5.5×10^-5 μg. CONCLUSION The method is accurate and sensitive. The study may provide a basis for the safety monitoring of formaldehyde and acetaldehyde.