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目的建立一种应用超高效液相色谱仪(UPLC)-FLD/PDA双检测器串联快速测定纸质食品包装材料中11种荧光增白剂的新型检测方法。方法样品经40%乙腈水溶液提取后,采用Waters ACQUITY UPLC BEH C_(18)柱(1.7μm,2.1 mm×100 mm)分离,流动相梯度洗脱,荧光检测器(FLD)激发波长350nm,发射波长430nm,二极管阵列检测器(PDA)350 nm波长,串联荧光和二极管阵列检测器进行双检测器定性定量测定。结果在纸杯、纸碗、纸盘、纸盒4种基质中,11种荧光增白剂得到良好分离,荧光检测器与二极管阵列检测器在25~1000 ng/m L线性范围内,相关系数均大于0.99,加标回收率为82.2%~104.1%,RSD均小于10%(n=6)。11种荧光增白剂检出限:荧光检测器为0.20~0.28 mg/kg,二极管阵列检测器为1.4~2.5 mg/kg。结论 UPLC-FLD/PDA法可以分离11种荧光增白剂,且峰形较好、回收率高、易于操作,是测定纸质食品包装材料中荧光增白剂的有效方法。
OBJECTIVE To establish a novel method for the rapid determination of eleven fluorescent whitening agents in paper food packaging materials by using ultra-high performance liquid chromatography (UPLC) -FLD / PDA dual detector. Methods After the sample was extracted with 40% acetonitrile, the sample was separated on a Waters ACQUITY UPLC BEH C 18 column (1.7 μm, 2.1 mm × 100 mm). The mobile phase was gradient elution. The excitation wavelength of the fluorescence detector (FLD) was 350 nm and the emission wavelength 430 nm, diode array detector (PDA) wavelength of 350 nm, tandem fluorescence and diode array detector for dual detector qualitative and quantitative determination. Results Among the four kinds of matrices such as paper cups, paper bowls, paper trays and cartons, 11 kinds of fluorescent whitening agents were well separated. The linearity range of fluorescence detector and diode array detector was 25 ~ 1000 ng / m L, the correlation coefficient Above 0.99, the spiked recoveries ranged from 82.2% to 104.1% with RSDs less than 10% (n = 6). The detection limits of 11 kinds of optical brighteners were 0.20 ~ 0.28 mg / kg for fluorescence detector and 1.4 ~ 2.5 mg / kg for diode array detector. Conclusion UPLC-FLD / PDA method can separate 11 kinds of optical brighteners, and the peak shape is good, high recovery, easy to operate, is an effective method for the determination of optical brightener in paper food packaging materials.