固相萃取-气相色谱-质谱联用对吸管纸中氯丙醇提取量的测定  

Determination of Chlorine Propanol in Straw Paper by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

作　　者：杜显生 宋元航 Du Xiansheng;Song Yuanhang(Mudanjiang Hengfeng Paper Co.,Ltd.,Mudanjiang 157013,Heilongjiang,China)

机构地区：[1]牡丹江恒丰纸业股份有限公司,黑龙江牡丹江157013

出　　处：《中华纸业》2021年第10期20-25,共6页China Pulp & Paper Industry

摘　　要：建立了食品接触用吸管纸在模拟萃取液中,对1,3-二氯-2-丙醇和3-氯-1,2-丙二醇提取量的测定方法。采用常温氯化钠水溶液浸泡制备模拟提取液,硅藻土固相萃取柱净化,乙醚-异辛烷溶液洗脱,流出物旋蒸浓缩,经七氟丁酰基咪唑衍生化,再通过气相色谱-质谱联用仪选择离子扫描分析,内标法定量。结果表明:1,3-二氯-2-丙醇和3-氯-1,2-丙二醇标准溶液浓度为0~200μg/L范围内线性关系较好,R2分别为0.9996、0.9999;方法的加标回收率分别为94.0%、105.1%;精密度偏差分别为4.6%、2.9%;在信噪比(S/N)为10的条件下,方法定量检出限(LOQ)为1.77μg/L、1.61μg/L。该方法具有定量准确、检出限低等优点,可完全满足吸管纸中1,3-二氯-2-丙醇和3-氯-1,2-丙二醇提取量的测试要求。A method which was used to detect the content of 1,3-dichloro-2-propanol and 3-monochloro-1,2-propanediol in simulated extractive liquid from food grade straw paper was established.The simulated extract was prepared by soaking in sodium chloride solution in 25℃,and then going through being purified by solid phase extraction column of diatomite,and eluted by ether and isooctane solution,and then concentrated by rotary evaporation,and derived by sevoflurbutadil imidazole.Then,the extraction liquid was analyzed by selective ion scanning and internal standard method by gas chromatogram and mass spectrometry.The results indicated that the linear relationship(R2)for 1,3-dichloro-2-propanediol and 3-monochloro-1,2-propanediol respectively was 0.9996 and 0.9999 which was quite great in the content range of 0~200 g/L.The standard recovery of the method was 94.0%and 105.1%separately.The precision deviation was 4.6%and 2.9%severally.When the signal-to-noise ratio(S/N)was 10,the LOQ of the method was 1.77μg/L and 1.61μg/L respectively.This method has lots of advantages including accurate quantif ication and low detection limit,especially satisf ying the test requirements of ext raction quantities of 1,3-dichloro-2-propanol and 3-monochloro-1,2-propanediol from straw paper.

关 键 词：吸管纸 固相萃取-气相色谱-质谱联用法 1 3-二氯-2-丙醇 3-氯-1 2-丙二醇 提取量 

分 类 号：TS77[轻工技术与工程—制浆造纸工程]