1.上海中医药大学 中药学院,上海 201203
2.上海市食品药品检验研究院,国家药品监督管理局 中药质量控制重点实验室,上海 201203
季申,博士,主任药师,研究方向:中药、天然药物及保健食品质量控制和安全性检测方法研究,E-mail:jishen2021@126.com
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李康,李丽敏,程益清等.基于HPLC-ICP-MS的海螵蛸中不同砷形态含量及其转移率研究[J].分析测试学报,2023,42(08):1000-1006.
LI Kang,LI Li-min,CHENG Yi-qing,et al.Investigation on Content and Transfer Rate of Different Arsenic Species in Sepiae Endoconcha Based on HPLC-ICP-MS[J].Journal of Instrumental Analysis,2023,42(08):1000-1006.
李康,李丽敏,程益清等.基于HPLC-ICP-MS的海螵蛸中不同砷形态含量及其转移率研究[J].分析测试学报,2023,42(08):1000-1006. DOI: 10.19969/j.fxcsxb.23042806.
LI Kang,LI Li-min,CHENG Yi-qing,et al.Investigation on Content and Transfer Rate of Different Arsenic Species in Sepiae Endoconcha Based on HPLC-ICP-MS[J].Journal of Instrumental Analysis,2023,42(08):1000-1006. DOI: 10.19969/j.fxcsxb.23042806.
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(As Ⅲ),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 spectrometry(HPLC-ICP-MS) was established for the determination of arsenic species in Sepiae Endoconcha.Research on the transfer rates of arsenic and arsenic species in Sepiae Endoconcha after decoction 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 exchange column by gradient elution,with 20 mmol/L and 100 mmol/L ammonium carbonate as the mobile 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 As Ⅲ was detected in only 1 batch.Moreover,3 kinds of unknown arsenic species were found in Sepiae Endoconcha.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 arsenic 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.
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 Endoconchaarsenic specieshigh performance liquid chromatography-inductively coupled plasma mass spectrometrycontent determinationtransfer rate
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