高效液相色谱法测定口腔清洁用品中铜叶绿酸二钠和铜叶绿酸三钠  

HPLC Determination of Chlorophyllin Copper Disodium and Chlorophyllin Copper Trisodium in Oral Cleaning Products

作　　者：于秋玲[1] YU Qiuling(Shaanxi Energy Institute, Xianyang 712000, China)

机构地区：[1]陕西能源职业技术学院,咸阳712000

出　　处：《理化检验（化学分册）》2018年第11期1339-1343,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：采用高效液相色谱法测定口腔清洁用品中铜叶绿酸二钠和铜叶绿酸三钠的含量。口腔清洁用品样品5.000 0g与pH 5.5的0.2mol·L^(-1)乙酸-乙酸铵缓冲溶液20mL混匀,加入5.0g吸附剂(聚酰胺粉)。离心后用20mL解吸液(0.1mol·L^(-1)氢氧化钠溶液和甲醇以体积比1∶10组成的混合液)解吸沉淀2次(每次10mL),合并上清液于45℃水浴蒸发至近干,加入1mL流动相A,经0.22μm有机微孔滤膜过滤。以YMC Carotenoid C_(30)色谱柱为固定相,将甲醇、水和甲酸以体积比90∶10∶0.1组成的混合液(A)和叔丁基甲醚、甲醇和甲酸以体积比100∶10∶0.1组成的混合液(B)以不同比例混合的溶液为流动相进行梯度洗脱,在检测波长405nm处进行测定。铜叶绿酸二钠和铜叶绿酸三钠的质量浓度均在5.0～500.0mg·L^(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为1.5μg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为89.6%～98.4%,测定值的相对标准偏差(n=6)为1.4%～2.7%。HPLC was applied to the determination of chlorophyllin copper disodium and chlorophyllin copper trisodium in oral cleaning products. The oral cleaning product sample （5.000 0 g） was mixed with 0.2 tool · L^- 1 acetic acid-ammonium acetate buffer solution of pH 5.5 （20 mL）, and then 5.0 g of adsorbent （polyamide） was added. After centrifugation, the precipitate was desorbed twice （10 mL each） with 20 mL of desorption solution （mixture of 0.1 mol · L^-1 NaOH solution and methanol with ratio of 1 .＂ 10）. The combined supernatant was evaporated to near dryness at 45 ℃ in the water bath. 1 mL of mobile phase A was added and then the solution was filtered on 0.22 μm organic rnicroporous membrane. YMC Carotenoid C30 chromatographic column was used as stationary phase, and the mixed solution of mixture （A） of methanol-water-formic acid （90＋10＋0.1） and mixture （B） of TBME-methanol-forrnic acid （100＋10＋0.1） mixed in different ratios was used as mobile phase in gradient elution. Detection at 405 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of chlorophyllin copper disodiurn and chlorophyllin copper trisodium were kept in the same range of 5.0-500.0 mg· L^- 1 , with same detection limit （3S/N） of 1.5 μg · kg^-1. On the base of blank sample, test for recovery was made by standard addition methods values of recovery found were in the range of 89.6%-98.4%, with RSDs （n=6） in the range of 1.4%-2.7%.

关 键 词：高效液相色谱法 口腔清洁用品 铜叶绿酸二钠 铜叶绿酸三钠 

分 类 号：O652.63[理学—分析化学]