HPLC Determination of Chlorophyllin Copper Disodium and Chlorophyllin Copper Trisodium in Oral Cleaning Products
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 0 g与pH 5.5的0.2 mol·L-1乙酸-乙酸铵缓冲溶液20 mL混匀,加入5.0 g吸附剂(聚酰胺粉)。离心后用20 mL解吸液(0.1 mol·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10 mL),合并上清液于45℃水浴蒸发至近干,加入1 mL流动相A,经0.22 μm有机微孔滤膜过滤。以YMC Carotenoid C30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405 nm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5.0~500.0 mg·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1.5 μg·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%。
Abstract
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 mol·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 microporous 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-formic 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 disodium 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 method; 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%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201811021
所属栏目 工作简报
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收稿日期 2018/1/5
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备注于秋玲,副教授,研究方向为分析化学,1947223160@qq.com
引用该论文: YU Qiuling. HPLC Determination of Chlorophyllin Copper Disodium and Chlorophyllin Copper Trisodium in Oral Cleaning Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(11): 1339~1343
于秋玲. 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[J]. 理化检验-化学分册, 2018, 54(11): 1339~1343
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【9】孔鲁裔.果酒中叶绿素铜钠的测定-分光光度法[J].生命科学仪器, 2008,6(1):48-53.
【10】孙志勇,沈兆雷.分光光度法测定牙膏中叶绿素铜钠盐的含量[J].口腔护理用品工业, 2012,22(3):23-25.
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