离子对反相色谱法研究（E）－4，4′－二氨基二苯乙烯－2，2′－二磺酸及其杂质组分

Studies on E-Isomer of 4,4’-Diaminostilbene-2,2’-Disulphonic Acid and Its Related Impurities by Paired-Ion Reversed-phase High Performance Liquid Chromatography(HPLC)

建立了离子对反相ＨＰＬＣ分离测定（Ｅ）－４，４′－二氨基二苯乙烯－２，２′二磺酸［（Ｅ）ＤＡＳ］及其中间产物和杂质组分的方法。解决了测定的稳定性问题，且各组分线性范围宽，检测限低。已用于工业样品的测定，结果令人满意。

-isomer of 4,4’-diaminostilbene-2,2’-disulphonic acid((E)DAS) is an important intermediate in themanufacture of dyes and fluorescent whitening agents。 The separation and determination of(E)-DAS and itsrelated impurities is important not only for quality control but also for process developrnent. In this work apaired-ion reversed-phase HPLC method was developed for quantitative determination of (E) DAS and mainby-products,specifically:Z-isomer of DAS,p- aminotoluene-2-sulphonic acid(PATS),p -nitrotoluene-2-sulphonic acid(PNTS).4,4’-diaminodibenzyl-2,2’-disulphonic acid(DADB)and 4,4’-dinitrostilbene-2.2’-disulphonic acid(DNS)etc。The separation wa5 performed by using a 4. 6mm i.d.×150mm Zorbax ODS col-umn packed with 5μm C_(18);an 1.0 mL/min eluent containing 0.05 mol /L aqueous hexade-cyltrimethylammonium bromide,0.02mol/L Tris (hydroxymethyl)aminomethane buffered to pH 7.0 withacetic acid and 75%(V/V) methanol,at column temperature of 40℃,and a UV spectrophotornetric detectorat 254 nm。 The calibration curve of all cornpoundS had good linearity over wide concentration range of about4.4× 10￣(-8)～16g/L,and the minimum detection limits at a signal-to-noise ratio of 3were about(1.0～4.4)ng.The method has been applied to the industrial qample testing with good results and reproducibility。