摘要
建立了高效液相色谱法(HPLC)和液相色谱-串联质谱法(LC-MS/MS)测定纺织品中分散黄23和分散橙149含量的方法。样品上的分散染料经氯苯蒸汽完全剥离纤维,浓缩后的残留物用甲醇定容,以0.1%H3PO4(或0.1%甲酸)和乙腈为流动相,经反相色谱柱分离后,用二极管阵列检测器(DAD)在420nm处测定,并用电喷雾串联质谱确认。分散黄23和分散橙149的定量离子对分别为m/z303/105和m/z459/399。分散黄23和分散橙149的检出限(S/N=3):HPLC法为2.0和1.0mg/kg,LC-MS/MS法都为1.0μg/kg。HPLC在0.5～250mg/L、LC-MS/MS在0.5～200μg/L范围内,线性相关系数都大于0.995。方法的回收率在92.1%～98.7%之间,批间RSD都小于8.0%,含有分散黄23的阳性样品重复测试的RSD也小于8.0%。
A high performance liquid chromatographic （HPLC） method and a liquid chromatography-tandem mass spectrometric （LC-MS/MS） method were developed to determine Disperse Yellow 23 （DY23） and Disperse Orange 149（DO149） in textile. The disperse dyes in textile fibres were completely extracted by chlo- robenzene. After removal of the solvent, the extract was dissolved in methanol and separated by reversed phase liquid chromatography containing acetontrile and 0.1% phosphate acid （or 0. 1% formic acid） solution as mobile phase, determined by diode array detector （DAD） at 420 nm, and confirmed by electrospray ioniza- tion-tandem mass spectrometer （ESI-MS/MS）- The quantification transitions of DY23 and DO149 were m/z 303/105 and m/z 459/399 respectively. Based on the calculation of signal to noise of 3, the limits of detec- tion of DY23 and DO149 were 2.0 and 1.0 mg/kg respectively for the HPLC method, and both 1.0 μg/kg for the LC-MS/MS method. Both the HPLC and LC-MS/MS methods provided better linearity （r 〉0. 995） at the range of 0.5 - 250 mg/L and 0.5 - 200 μg/L respectively. In recovery experiments, all recovery rate was 92.1% -98.7% and all relative standard deviation （RSD） were less than 8.0%. On repeatable experiments on positive samples, RSD of detection results of DY23 was also less than 8.0%
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2008年第9期1289-1292,共4页
Chinese Journal of Analytical Chemistry
基金
"十一五"国家科技支撑计划重点项目(No.2006BAK10B03-3)资助
关键词
纺织品
分散黄23
分散橙149
高效液相色谱
液相色谱-串联质谱
Textile, disperse yellow 23, disperse orange 149, high performance liquid chromatography, liquid chromatography-tandem mass spectrometry
