超高效合相色谱法快速检测纺织品中的8种荧光增白剂

建立了同时检测纺织品中1,2-双(5-甲基-2-苯并恶唑基)-乙烯(PF)、7-二乙氨基-4-甲基香豆素(SWN)、2,2'-(2,5-二苯基硫代)双5-(1,1-二甲基乙基)]苯并恶唑(OB)、2-4-2-4-(2-苯并恶唑基)苯基]乙烯基]苯基]-5-甲基苯并恶唑(KSN)、1,4-双(2-氰基苯乙烯基)苯(ER-Ⅰ)、1-邻氰苯乙烯基-4-对氰苯乙烯基苯(ER-Ⅱ)、2,2-(1,4-亚萘基)双(苯并恶唑)(KCB)和4,4'-双2-(2-甲氧基苯基)亚乙基]-1,1'-联苯(FP)8种荧光增白剂的超高效合相色谱(UPC²)检测方法。样品经二甲苯提取、浓缩、定容后,由UPC²进行定性定量分析。以超临界CO₂-甲醇为流动相,梯度洗脱,采用ACQUITY UPC² HSS C18 SB色谱柱(100 mm×3.0 mm,1.8 μm)进行分离。8种荧光增白剂在1.0~20.0 mg/L范围内线性良好(r≥0.9991),定量限(LOQ,S/N=10)在0.70~0.95 mg/L之间。不同添加水平的回收率范围为90.9%~96.5%,相对标准偏差(RSD)为2.8%~4.2%。该方法简单、准确度高、分析时间短,可用于快速检测纺织品中的8种荧光增白剂。

Rapid detection of eight fluorescent whitening agents in textile by ultra performance convergence chromatography

An accurate quantitative and confirmative method has been developed for the determination of eight fluorescent whitening agents (FWAs) in textile by ultra performance convergence chromatography (UPC²) coupled with photo diode array (PDA) detection, including 1,2-bis(5-methyl-2-benzoxazole)ethylene (PF), 7-diethylamino-4-methylcoumarin (SWN), 2,2'-(2,5-thiophenediyl)bis(5-(1,1-dimethylethyl)-benzoxazol (OB), 2-4-2-4-(2-benzoxazolyl) phenyl]ethenyl]phenyl]-5-methyl-benzoxazol (KSN), 1,4-bis(2-cyanostyryl)benzene (ER-Ⅰ), 1-(2-cyanostyryl)-4-(4-cyanostyryl)benzene (ER-Ⅱ), 2,2'-(1,4-naphthalenediyl)bis-benzoxazol (KCB), 4,4'-bis2-(2-methoxyphenyl)ethenyl]-1,1'-biphenyl (FP). The sample was extracted with xylene and concentrated by a rotary evaporator, and then qualitatively and quantitatively analyzed by UPC². The separation of target compounds was achieved on an ACQUITY UPC² HSS C18 SB column (100 mm×3.0 mm, 1.8 μm) by a gradient elution with supercritical carbon dioxide and methanol as mobile phases. External standard method was used for the quantitative determination and the calibration curves showed good linearity in the concentration range of 1.0-20.0 mg/L for the eight target compounds with correlation coefficients not less than 0.9991. The limits of quantification of the eight compounds (LOQs, S/N=10) were 0.70-0.95 mg/L. The average recoveries of the eight compounds ranged from 90.9% to 96.5% at the spiked levels of 2.0, 5.0, 10.0 mg/kg with the relative standard deviations (RSDs) of 2.8%-4.2%. The method is simple, accurate and time-saving with high sensitivity, and can be used for the rapid determination of the eight FWAs in textile.