固相萃取-离子排斥色谱法测定爽身粉中硼酸和硼酸盐的含量  

Determination of Boric Acid and Borate in Talcum Powder by Solid Phase Extraction-Ion Exclusion Chromatography

作　　者：陈岑 黄柳倩 高艳琳 程巧鸳 颜琳琦[1] CHEN Cen;HUANG Liuqian;GAO Yanlin;CHENG Qiaoyuan;YAN Linqi(Zhejiang Institute for Food and Drug Control,Hangzhou 310052,Zhejiang,China;Zhejiang Chinese Medical University,Hangzhou 310053,Zhejiang,China)

机构地区：[1]浙江省食品药品检验研究院,浙江杭州310052 [2]浙江中医药大学,浙江杭州310053

出　　处：《香料香精化妆品》2023年第5期138-142,共5页Flavour Fragrance Cosmetics

摘　　要：创建了固相萃取-离子排斥色谱法测定爽身粉中硼酸和硼酸盐的方法。样品纯水提取,过OnGuard II RP固相萃取小柱净化,以IonPac ICE-borate离子排斥柱为色谱柱,淋洗液为2.5 mmol/L甲基磺酸-60 mmol/L甘露醇,25 mmol/L四甲基氢氧化铵-15 mmol/L甘露醇为抑制器再生液,抑制型电导检测器检测。结果表明,硼酸在1~200μg/mL范围内具有良好的线性关系,相关系数(R2)为1.0000,检出限为32.7 mg/kg,定量限为62.9 mg/kg,均低于标准规定检出限和定量限。加标回收率为95.6%~104.0%,相对标准偏差(n=6)为0.60%~1.68%。该方法专属性强,重现性好,准确度高,可满足爽身粉产品中硼酸和硼酸盐的检测需求。A method was developed to determine boric acid and borate in talcum powder by solid phase extraction-ion exclusion chromatography.Samples were extracted with water,and cleaned up by the OnGuard II RP column.Chromatographic separation was performed on IonPac ICE-borate ion exclusion column with the solution of 2.5 mmol/L methylsulfonic acid and 60 mmol/L mannitol as eluent and the solution of 25 mmol/L tetramethylammonium hydroxide and 15 mmol/L mannitol as regenerant,respectively.The detection was performed by suppressed conductive detector.The results showed that the borate acid had a good linear relationship in 1-200μg/mL with the correlation coefficient(R2)was 1.0000.The limits of detection of this method(LOD)was 32.7 mg/kg,and the limits of quantification(LOQ)was 62.9 mg/kg,which were all lower than LOD and LOQ of the standard method.The standard recoveries were 95.6%-104.0%,and the relative standard deviations(n=6)were 0.60%-1.68%.This method is specific,repeatability and accuracy,and suitable for the detection requirements for the determination of boric acid and borate in talcum powder.

关 键 词：爽身粉 硼酸和硼酸盐 离子排斥色谱法 固相萃取 

分 类 号：O657.7[理学—分析化学] TQ658[理学—化学]