基于织物相吸附萃取技术测定藿香正气水中浸出物及风险评估
Detection of Leachables in Huoxiang Zhengqi Liquid Based on Fabric Phase Sorptive Extraction and Their Risk Assessment
- 分析测试学报 2021年40卷第12期 页码：1681-1689
- 作者机构：
1.北京化工大学 化学学院，北京 100029
2.首都医科大学 基础医学院，北京 100069
- 作者简介：
杜振霞，博士，教授，研究方向：分析化学，E－mail：duzx@mail.buct.edu.cn
- 基金信息：国家自然科学基金项目(21874006)
DOI：10.19969/j.fxcsxb.21032203
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杨雨希,康天惠,孙雪纯等.基于织物相吸附萃取技术测定藿香正气水中浸出物及风险评估[J].分析测试学报,2021,40(12):1681-1689.
YANG Yu-xi,KANG Tian-hui,SUN Xue-chun,et al.Detection of Leachables in Huoxiang Zhengqi Liquid Based on Fabric Phase Sorptive Extraction and Their Risk Assessment[J].Journal of Instrumental Analysis,2021,40(12):1681-1689.
杨雨希,康天惠,孙雪纯等.基于织物相吸附萃取技术测定藿香正气水中浸出物及风险评估[J].分析测试学报,2021,40(12):1681-1689. DOI： 10.19969/j.fxcsxb.21032203.
YANG Yu-xi,KANG Tian-hui,SUN Xue-chun,et al.Detection of Leachables in Huoxiang Zhengqi Liquid Based on Fabric Phase Sorptive Extraction and Their Risk Assessment[J].Journal of Instrumental Analysis,2021,40(12):1681-1689. DOI： 10.19969/j.fxcsxb.21032203.
摘要
采用织物相吸附萃取技术（FPSE）结合超高效液相色谱－串联质谱（UPLC－MS/MS）建立了藿香正气水中包装材料浸出物的分析方法。通过溶胶－凝胶法将聚二甲基硅氧烷（PDMS）涂覆在纯棉纤维布上制备织物萃取相。优化了影响萃取效率的关键因素，确定在5 mL样品溶液中放置2.0 cm × 2.0 cm的织物萃取相和磁力搅拌子，以700 r/min萃取30 min，1 mL乙腈作为反萃取溶剂超声洗脱10 min，可获得最佳萃取效果。结果显示，该方法线性关系良好，相关系数,r, ≥ 0.996 1，检出限（LOD）为0.5～1.5 μg/L，定量下限（LOQ）为1.5～4.0 μg/L。8种分析物的加标回收率为73.8%～98.2%，相对标准偏差（RSD，,n, = 3）为0.98%～8.4%。选择乙醇/水（1∶1）、异丙醇2种浸泡液对藿香正气水塑料包装瓶进行模拟提取，采用超高效液相色谱－四极杆飞行时间质谱（UPLC－QTOF MS）检测，通过基于UNIFI软件的聚合物添加剂谱库和联网筛查方式对可提取物进行快速筛查，然后利用UPLC－MS/MS靶向检测霍香正气水中的浸出物，检出了4种浸出物并对其进行定量分析。基于Toxtree软件和T.E.S.T软件的风险评估结果显示，4种浸出物的每日摄入量均未超过成人每日允许暴露量，说明藿香正气水中的浸出物含量是相对安全的。
Abstract
A new method for the rapid detection of leachables in Huoxiang Zhengqi liquid was developed by ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with fabric phase sorptive extraction（FPSE）．The fabric extraction phase was prepared by coating polydimethylsiloxane（PDMS） on the cotton fiber cloth through a sol－gel reaction．Effects of extraction time，ionic strength，type of desorption solution，volume of desorption solution and desorption time on extraction efficiency were optimized．A 2.0 cm × 2.0 cm fabric extraction phase and magnetic agitator were placed in a 5 mL sample，extracted for 30 min at 700 r/min，then ultrasonically eluted with 1 mL acetonitrile as the back-extraction solvent for 10 min to obtain the best extraction effect．The results showed that the calibration curves for the analytes showed good linearity with their correlation coefficients（,r,） not less than 0.996 1．The limits of detection（LOD） and limits of quantitation（LOQ） were in the ranges of 0.5－1.5 μg/L and 1.5－4.0 μg/L，respectively．Spiked recoveries for 8 analytes were in the range of 73.8%－98.2%，with relative standard deviations（RSD，,n, = 3） of 0.98%－8.4%．In order to simulate the solvent formula of Huoxiang Zhengqi liquid，ethanol/water（1∶1） was selected to extract the plastic packaging bottles．Moreover，in order to get a more reliable and comprehensive extractables profile，isopropanol was also used as the storage solution to obtain an extremely harsh environment．The sample was detected by ultra-performance liquid chromatography－quadrupole time-of-flight mass spectrometry（UPLC－QTOF MS），and the extractables of the sample were screened through the UNIFI software based on a polymer additive library and online screening．There were 33 compounds identified．Then these extractables were targetedly detected in the Huoxiang Zhengqi liquid by UPLC－MS/MS．A total of 4 leachables were detected and quantified．The results of toxicological evaluation based on Toxtree and T.E.S.T software showed that the actual daily intake of the 4 leachables will not exceed the permitted daily exposure，indicating that the content of leachables in Huoxiang Zhengqi liquid is relatively safe．
关键词
药品包装材料可提取物与浸出物织物相吸附萃取技术（FPSE）快速筛查风险评估超高效液相色谱－串联质谱
Keywords
pharmaceutical packaging materialsextractables and leachablesfabric phase sorptive extraction（FPSE）fast screeningrisk assessmentultra-performance liquid chromatography－tandem mass spectrometry
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