日化用多糖产品中阳离子醚化剂残留量的检测  

Determination of residual QUAB reagents in cationic polysaccharides in personal care products

作　　者：孙雪莲 周利英[1,2] 朱明山 何建平 邓明宇[1,3] 尹恒 何俊 

机构地区：[1]昆山京昆油田化学科技开发公司,江苏昆山215300 [2]昆山出入境检验检疫局,江苏昆山21530 [3]苏州大学材料与化学化工学部,江苏苏州21512

出　　处：《化学研究与应用》2014年第6期946-950,共5页Chemical Research and Application

基　　金：江苏省自然科学基金项目(BK2009581)资助

摘　　要：通过高效液相色谱仪联用线性离子阱质谱建立了阳离子多糖产品中醚化剂残留量的检测方法。以阳离子瓜尔胶为例,采用硼砂-NaOH水溶液对残留醚化剂进行了提取,以C18为分析色谱柱,甲醇-水（0．1%三氟乙酸TFA）作为流动相进行梯度洗脱分离。质谱采用电喷雾正离子（ ESI＋）电离模式,选择反应检测（ SRM）模式检测。结果表明：QUAB-151和QUAB-188在0．5~100μg·mL-^1范围内呈良好的线性关系,相关系数（ r2）均大于0．998．检出限分别为0．12和0．14μg·mL-^1,定量限分别为0．39和0．46μg·mL-^1。从0．5~100μg·mL-^1的添加浓度的检测结果可以看出,平均回收率均在99．6%~103．2%之间,相对标准偏差（RSD,n=3）均为3．51%以下。该方法操作简便快速,定量准确,可适用于化妆品中QUAB-151和QUAB-188的残留测定。A high performance liquid chromatography-tandem mass spectrometry method was established for the determination of re-sidual QUAB reagents in cationic guar gum. The analyte was extracted with borax-NaOH aqueous solution,then separated on a C18 column in gradient elution mode using methanol and water（ with 0. 1%TFA） as mobile phase,and finally detected with positive elec-trospray ionization（ ESI＋） in selective reaction monitoring（ SRM） mode. The calibration curves of QUAB-151 and QUAB-188 showed good linearity within the range of 0. 5-100μg＆#183;mL-1 with the correlation coefficients（ r2 ） greater than 0. 998. The limits of detection （LOD）were 0. 12 and 0. 14μg·mL-^1 respectively,and the limits of quantification（LOQ）were 0. 39 and 0. 46μg·mL-^1corre-spondingly. The recoveries of the analyte in guar gum were 99. 6%-103. 2%at the spiked levels of 0. 5-100μg·mL-^1 . The relative standard deviations（RSD,n=3）were less than 3. 51%. This method were easy,fast and accurate,and also can be used for determi-nation of residual QUAB reagents in other cationic polysaccharides.

关 键 词：液质 多糖 醚化剂残留量 检测 

分 类 号：O657.7[理学—分析化学]