IP-HPLC法测定织物中致癌染料含量  

Determination of carcinogenic dyestuffs in textiles by IP-HPLC method

作　　者：丁友超[1] 蔡建和[1] 杨锦富[1] 曹锡忠[1] 杨安南[1] 

机构地区：[1]江苏出入境检验检疫局,江苏南京210001

出　　处：《印染》2008年第15期38-41,共4页China Dyeing and Finishing

基　　金："十一五"国家科技支撑计划重点项目;出入境检验检疫安全关键技术研究(项目编号:2006BAK10B03)

摘　　要：采用不同试剂蒸汽作为剥色剂剥离织物纤维上的染料，用离子对反相液相色谱法（IP-HPLC）对不同织物上的9只禁用染料同时进行测定。用吡啶／水（4／3，v／v）、吡啶／甲酸／水（20／5／75，v／v）和氯苯可分别完全剥离天然纤维上的直接染料和酸性染料，腈纶纤维上的碱性染料和涤纶纤维上的分散染料。以磷酸二氢四丁基铵作为阳离子对试剂，以增加阴离子染料的保留，在反相色谱柱上通过乙腈洗脱，可完全分离这9只染料，再用二极管阵列检测器在最大吸收波长检测染料含量。该方法中，9只禁用染料的定量限为1．0—10．0mg／kg，线性相关系数都大于0．995，回收率为92．3％-106．8％，批间的相对标准偏差（RSD）均小于10．0％。This paper developed a method by full extraction with the vapor of color stripping reagent and accurate determination with ion-pair reversed-phase high performance liquid chromatography （IP-HPLC） to quantify the content of carcinogenic dye- stuffs in textiles. The mixture reagent of pyridine/water（4/3,v/v） was used to strip direct and acid dyestuffs from the cellulose and protein fibers, while pyridine/formic acid/water（20/5/75,v/v） was used to strip basic dyestuff from acrylic fiber and chlo- robenzene was used to strip disperse dyestuff from polyester and other chemical fibers. The nine dyestuffs could be separated well on a reversed-phase C18 column with acetonitrile as elution solvent and tetrabutylamine phosphate as ion-pair reagent used to improve the chromatographic retention of negative-ionic direct and acid dyestuffs. The dyestuffs were detected by diode array detector （DAD） and quantified at the wavelength close to the maximum absorbance in visual region. Based on the calculation of signal to noise of 10, limits of quantification （LOQ） was 1.0 -10.0mg/kg. The method was evaluated with better linearity （11 〉 0.995 ）, acceptable recovery ratio （92.3 % - 106.8 % ） and satisfactory robustness （ all RSD 〈 10. 0% ）. The application of the method was demonstrated on six reference samples with all RSD less than 9.3%.

关 键 词：测试 含量 致癌染料 液相色谱法 

分 类 号：TS197[轻工技术与工程—纺织化学与染整工程]