摘要
建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)测定海螵蛸药材中多种砷形态的分析方法,并研究了海螵蛸药材煎煮后砷及砷形态的转移率。样品采用0.02 mol/L乙二胺四乙酸二钠(EDTA-2Na)溶液超声提取60 min,以Dionex IonPac As7阴离子交换柱为色谱柱,2 mmol/L和100 mmol/L碳酸铵溶液为流动相进行梯度洗脱。结果显示,27批海螵蛸药材中均检出砷甜菜碱(As B)和砷胆碱(As C),其中26批检出二甲基砷(DMA),10批检出一甲基砷(MMA),1批检出微量亚砷酸(AsⅢ),并发现3个未知砷形态;海螵蛸药材水煎煮后砷及砷形态的平均转移率均大于50%,且存在个体差异。该方法准确度高,专属性好,明确了海螵蛸药材中砷形态的分布规律,并揭示了海螵蛸药材在煎煮过程中砷及砷形态的转移规律,可为海螵蛸药材的安全性评价奠定基础。
A high performance liquid chromatography-inductively coupled plasma mass spectrome-try(HPLC-ICP-MS)was established for the determination of arsenic species in Sepiae Endocon-cha.Research on the transfer rates of arsenic and arsenic species in Sepiae Endoconcha after decoc-tion was carried out.All samples were extracted with 0.02 mol/L EDTA-2Na solution by ultrasonic extraction for 60 min,and the arsenic species were separated on a Dionex IonPac As7 anion ex-change column by gradient elution,with 20 mmol/L and 100 mmol/L ammonium carbonate as the mo-bile phases.The results showed that As B and As C were detected in total 27 batches of samples,in which DMA was detected in 26 batches,MMA was detected in 10 batches and trace AsⅢwas de-tected in only 1 batch.Moreover,3 kinds of unknown arsenic species were found in Sepiae Endocon-cha.The average transfer rates for arsenic and arsenic species were more than 50%,which varied in different batches.With high accuracy and specificity,the method clarified the distributions of arse-nic species in Sepiae Endoconcha,revealing the transformations of arsenic and arsenic species,and it could lay a foundation for the safety evaluation of Sepiae Endoconcha.
作者
李康
李丽敏
程益清
周如洁
胡青
毛秀红
季申
LI Kang;LI Li-min;CHENG Yi-qing;ZHOU Ru-jie;HU Qing;MAO Xiu-hong;JI Shen(School of Pharmacy,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;National Medical Products Administration Key Laboratory for Quality Control of Traditional Chinese Medicine,Shanghai Institute for Food and Drug Control,Shanghai 201203,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第8期1000-1006,共7页
Journal of Instrumental Analysis
基金
上海市中药和保健食品品质与安全检测专业技术服务平台(21DZ2290200)
2023年度国家药品标准提高项目(2023Y14)。
关键词
海螵蛸
砷形态
高效液相色谱-电感耦合等离子体质谱
含量测定
转移率
Sepiae Endoconcha
arsenic species
high performance liquid chromatography-inductively coupled plasma mass spectrometry
content determination
transfer rate
