【摘要】：采用超高效液相色譜-四極桿飛行時間質(zhì)譜(UPLC-QTOF-MS),結(jié)合基于UNIFI軟件建立的174種聚合物添加劑的譜庫,實現(xiàn)了塑料藥品包裝材料中難揮發(fā)可溶出物(Extractables)的快速篩查和準確定量。樣品經(jīng)氯仿萃取后,以甲醇和0.1%甲酸水溶液為流動相在CORTECS C18(2.1 mm×100 mm,1.6μm)色譜柱上進行分離,在質(zhì)譜電噴霧正離子模式下,UPLC-QTOF-MS進行篩查和定量分析。結(jié)果表明,浸泡60 d緩沖鹽(25℃)中檢出4種物質(zhì),利用譜庫篩查確定其中1種物質(zhì)是鄰苯二甲酸二異癸酯(DIDP),采用外標法定量,測得其溶出量為1.98μg/L;其余3種物質(zhì)可通過精確質(zhì)量數(shù)、MSE譜圖等進行推斷定性,利用結(jié)構(gòu)與質(zhì)量數(shù)相近的鄰苯二甲酸二環(huán)己酯(DCHP)為內(nèi)標進行定量,3種提取物的總含量為10.80μg/L。利用DIDP進行回收率實驗,5,10,20μg/L 3個加標水平的回收率為90.1%~97.1%,相對標準偏差(RSD,n=6)不大于3.7%。該方法快速、準確、靈敏,適用于藥品包裝材料的安全性考察。
[Abstract]:The rapid screening and accurate quantification of volatile soluble substance (Extractables) in plastic medicine packaging materials were achieved by using ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) combined with the spectrum library of 174 kinds of polymer additives based on UNIFI software. The samples were extracted by chloroform and separated on CORTECS C18 (2.1 mm 脳 100 mm,1.6 渭 m) column with methanol and 0.1% formic acid solution as mobile phase. The UPLC-QTOF-MS was screened and quantitatively analyzed by mass spectrometry electrospray positive ion mode. The results showed that four substances were detected in 60 d buffer salt (25 鈩，

本文編號：2269287