染整助剂中残留有害有机溶剂的检测

Detection of harmful organic solvents residues in dyeing and finishing auxiliaries

建立了气相色谱-质谱联用法和高效液相色谱法测定染整助剂中N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)和1-甲基-2-吡咯烷酮(NMP)3种有害有机溶剂的方法。以甲醇作为萃取溶剂,样品经常温超声波萃取,萃取液直接进气相色谱-质谱联用仪和高效液相色谱仪进行分析。DMF、DMAc和NMP气相色谱-质谱法和高效液相色谱法的线性范围分别为0.5~30.0 mg/kg和0.25~10.00 mg/kg,气相色谱-质谱法和高效液相色谱法的定量限分别是0.50mg/kg和0.25 mg/kg。3种有机溶剂回收率在94.7%~100%,相对标准偏差均小于8.3%(n=10),符合残留物分析的技术指标要求。

An analytical method for the determination of 3 harmful organic solvents of N, N-dimethylforma （DMF） ,N, N-dimethylacetam（DMAc） and 1-methyl-2-pyrrolidone （NMP） in dyeing and finishing auxilia- ries is established by using gas chromatography-mass spectrometry （GC-MS） and high performance liq- uid chromatography（HPLC）. The samples are extracted by ultrasonic with methanol as extraction solvent at constant temperature, and the extraction liquid is analyzed by GC-MS or HPLC directly. The linear ranges of DMF, DMAc and NMP are 0.5N30 mg/kg and 0.25-10 mg/kg respectively. The limits of quantitation for GC-MS or HPLC are 0.5 mg/kg or 0.25 mg/kg respectively. The recovery rate of 3 organic solvents is 94.7%-100%, and the relative standard deviations are all less than 8.3% （n=10）.