液相色谱-离子阱-飞行时间串联质谱法高通量测定聚对苯二甲酸乙二醇酯塑料瓶中10种紫外吸收剂

High throughput determination of 10 kinds of ultraviolet stabilizers in polyethylene terephthalate plastic bottles by liquid chromatography-ion trap-time of flight mass spectrometry

目的建立了液相色谱-离子阱-飞行时间串联质谱法(liquid chromatography-ion trap-time of flight mass spectrometry,LCMS-IT-TOF)高通量快速测定聚对苯二甲酸乙二醇酯(polyethylene terephthalate,PET)塑料瓶中10种紫外吸收剂的方法。方法样品采用三氯甲烷浸泡,超声萃取,甲醇-乙腈混合液(3:2,V:V)辅助沉淀净化后用Shim-pack XR-ODS(50 mm×2.0 mm,1.6μm)色谱柱分离,0.1%甲酸水(V:V)和含0.1%甲酸的甲醇-乙腈混合液(3:2,V:V)为流动相进行梯度洗脱。采用电喷雾正离子模式监测,外标法定量。结果 10种紫外稳定剂在0.05~50μg/m L范围内线性关系良好,线性相关系数(r^2)均大于0.99;检出限为0.05~0.1 mg/kg;3个水平下的加标回收率为91.2%~103.4%;相对标准偏差(RSD)为1.2%~6.6%。结论该方法操作简便、快速、准确,可用于PET塑料瓶中10种紫外吸收剂的同时检测。

Objective To establish a method for high throughput determination of 10 kinds of ultraviolet stabilizers in polyethylene terephthalate（PET） plastic bottle by liquid chromatography-ion trap-time of flight mass spectrometry（LCMS-IT-TOF）. Methods The samples were extracted by trichloromethane and ultrasonic, and purified by methanol and acetonitrile mixture solution（3：2, V：V）. The separation of target compounds was carried out on a Shim-pack XR-ODS（50 mm×2.0 mm, 1.6 μm） column using water containing 0.1%（V：V） formic acid and methanol-acetonitrile mixture solution（3：2, V：V） as the mobile phases by gradient elution. The identification of the analytes was achieved in positive electrospray ionization source and quantification was carried out by external standard method. Results The results showed that the standard curves were obtained with good correlation coefficients（r2〉0.99） in the range of 0.05~50 μg/m L. The limits of detection（LODs, S/N=3） for 10 kinds of ultraviolet stabilizers were in the range of 0.05~0.1 mg/kg. The mean recoveries for the 10 ultraviolet stabilizers at 3 spiked levels were 91.2%~103.4% with relative standard deviation（RSD） of 1.2%~6.6%. Conclusion This method is simple, rapid, and accurate for the high throughput determination of 10 kinds of ultraviolet stabilizers in PET plastic bottles.