顶空固相微萃取-气相色谱质谱快速测定聚酰胺环氧氯丙烷湿强剂中氯丙醇含量

Rapid Determination of Chloropropanol in Wet Strength Agent by Headspace Solid Phase Microextraction and Gas Chromatography Mass Spectrometry

关键词:  1,3-二氯-2-丙醇  3-氯-1,2-丙二醇  纸和纸板  湿强剂  顶空固相微萃取

Key Words:1, 3-dichloro-2-propyl alcohol  3-chloro-1, 2-propylene glycol  paper and paperboard  wet strength agent  headspace solid phase microextraction

摘要:建立了快速测定聚酰胺环氧氯丙烷（PAE）湿强剂中1,3-二氯-2-丙醇和3-氯-1,2-丙二醇的顶空固相微萃取-气相色谱质谱方法。采用二乙烯基苯/碳宽范围/聚二甲基硅氧烷（DVB-CWR-PDMS）萃取头，取样量2 mL、萃取温度60 ℃、萃取时间30 min、加热器转速300 r/min、解析时间2 min、NaCl加入量1.2 g，对湿强剂氯丙醇进行萃取，经DB-WAX色谱柱（30 m×0.25 mm×0.25 μm）分离后，质谱选择离子监测模式检测，外标法定量。PAE湿强剂中1,3-二氯-2-丙醇和3-氯-1,2-丙二醇线性范围分别为0.01~0.1 mg/L和1.0~10 mg/L、相关系数均大于0.999、加标回收率范围分别为95%~110%和96%~113%、检出限分别为0.0001 mg/L和0.1 mg/L。该方法简单、准确、检出限低、无需使用衍生剂，大幅缩短前处理时间和成本，适用于PAE湿强剂样品中氯丙醇的快速测定。

Abstract:A rapid determination method of 1, 3-dichloro-2-propyl alcohol and 3-chloro-1, 2-proplylene glycol in polyamide-epichl-orohydrin（PAE） wet strength agents was developed by headspace solid phase microextraction-gas chromatography mass spectrometry. The optimized conditions were that using Divinylbenzene/Carbon Wide Range/Polydimethylsiloxane （DVB-CWR-PDMS） extraction head， under the conditions of sampling volume 2 mL at extraction temperature of 60 ℃ with extraction time for 30 min， heater speed of 300 r/min， analytical time of 2 min and NaCl addition amount of 1.2 g， the wet strength agent chloropropanol was extracted. DB-WAX column （30 m×0.25 mm×0.25 μm） was separated and detected by ion monitoring mode selected by mass spectrometry， and quantified by external standard method. The linear ranges of 1, 3-dichloro-2-propyl alcohol and 3-chloro-1, 2-propylene glycol in PAE were 0.01~0.1 mg/L and 1.0~10 mg/L， respectively， the correlation coefficients were greater than 0.999， the recoveries were 95%~110% and 96%~113%， and the detection limits were 0.0001 mg/L and 0.1 mg/L， respectively. The method was simple， accurate， low detection limit， without derivatives， greatly reduced the pretreatment time and cost， and was suitable for the rapid determination of chloropropanol in PAE wet strength agent samples.