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

作　　者：张竞帆 赵世鑫 温建宇 高君 ZHANG Jingfan;ZHAO Shixin;WEN Jianyu;GAO Jun(Sinolight Paper Inspection&Certification Co.,Ltd.,Beijing,100020;National Paper Quality Inspection and Testing Center,Beijing,100020)

机构地区：[1]中轻纸品检验认证有限公司,北京100020 [2]国家纸张质量检验检测中心,北京100020

出　　处：《中国造纸》2023年第11期109-115,共7页China Pulp & Paper

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×0.25μm)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。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 condi⁃tions 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×0.25μm)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,re⁃spectively,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 pre⁃treatment time and cost,and was suitable for the rapid determination of chloropropanol in PAE wet strength agent samples.

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 

分 类 号：TS727[轻工技术与工程—制浆造纸工程] TQ317.4[化学工程—高聚物工业]