Rapid Determination of 4 Aflatoxins in Chinese Medicinal Materials Based on Automated Immunomagnetic Bead Purification Technique

HUANG Xiao-jing; CHEN Su-yun; ZHOU Heng; WANG Jiang; GUO Qi; WANG Xiong; HU Qing; JI Shen

doi:10.12452/j.fxcsxb.23112513

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Rapid Determination of 4 Aflatoxins in Chinese Medicinal Materials Based on Automated Immunomagnetic Bead Purification Technique

Scientific Papers | 更新时间：2024-04-18

- Rapid Determination of 4 Aflatoxins in Chinese Medicinal Materials Based on Automated Immunomagnetic Bead Purification Technique
- Journal of Instrumental Analysis Vol. 43, Issue 4, Pages: 622-629(2024)
- 作者机构：
  
  1.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
  2.北京中检维康生物技术有限公司，北京 100044
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23112513
  CLC： O657.7;R282.6
- Published：15 April 2024，
  
  Received：25 November 2023，
  
  Revised：03 January 2024，
- 稿件说明：
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黄晓静,陈素云,周恒等.基于全自动免疫磁珠净化技术快速测定中药材中4种黄曲霉毒素[J].分析测试学报,2024,43(04):622-629.

HUANG Xiao-jing,CHEN Su-yun,ZHOU Heng,et al.Rapid Determination of 4 Aflatoxins in Chinese Medicinal Materials Based on Automated Immunomagnetic Bead Purification Technique[J].Journal of Instrumental Analysis,2024,43(04):622-629.
黄晓静,陈素云,周恒等.基于全自动免疫磁珠净化技术快速测定中药材中4种黄曲霉毒素[J].分析测试学报,2024,43(04):622-629. DOI： 10.12452/j.fxcsxb.23112513.

HUANG Xiao-jing,CHEN Su-yun,ZHOU Heng,et al.Rapid Determination of 4 Aflatoxins in Chinese Medicinal Materials Based on Automated Immunomagnetic Bead Purification Technique[J].Journal of Instrumental Analysis,2024,43(04):622-629. DOI： 10.12452/j.fxcsxb.23112513.

摘要

基于全自动免疫磁珠净化前处理技术，建立了适用于多种中药材基质中4种黄曲霉毒素的快速测定方法。中药材中的黄曲霉毒素经乙腈-水（9∶1）提取后，采用免疫磁珠自动富集净化后，由0.5%乙酸甲醇洗脱后定容；经Inertsil ODS-3 C

柱（250 mm×4.6 mm，5 μm）分离，以乙腈-甲醇-水为流动相等度洗脱，采用高效液相色谱-荧光检测器（HPLC-FLD）测定。以5种易污染黄曲霉毒素的中药材基质进行方法学验证。结果表明该方法的线性关系良好，相关系数（

）均达到0.999 9；检出限为0.06~0.2 μg·kg

-1

，定量下限为0.12~0.40 μg·kg

-1

；不同基质中的平均回收率为71.9%~116%，相对标准偏差为0.10%~6.9%；在18 min内可完成24批样品的净化，比免疫亲和柱法的检测效率提高近85%。该方法快速、准确，通用性强，可用于多种中药材中4种黄曲霉毒素的批量快速测定。

Abstract

A rapid method for the determination of four aflatoxins in various Chinese medicinal materials（CMMs） was established by fully automated immunomagnetic bead purification technology. Aflatoxins in CMMs were efficiently extracted by acetonitrile-water（9∶1），followed by enrichment and purification program of immuno-magnetic beads，with elution accomplished by methanol containing 0.5% acetic acid. Separation was achieved on an Inertsil ODS-3 C

column （250 mm × 4.6 mm，5 μm） with a mobile phase consisting of acetonitrile，methanol，and water. Isocratic elution was operated with a flow rate of 1.0 mL·min

-1

and analyzed by high performance liquid chromatography-fluorescence detector（HPLC-FLD）. The method was validated and applied to five CMMs matrices known to be susceptible to aflatoxin contamination. The method had a good linear relationship with correlation coefficients（

） all reach 0.999 9. The limits of detection were 0.06-0.2 μg·kg

-1

and the limits of quantitation were 0.12-0.40 μg·kg

-1

. The average recoveries in different matrices were 71.9%-116%，with the relative standard deviations ranging of 0.10%-6.9%. The automated method takes less than 18 min to finish the batch purification of 24 samples. It appeared an outstanding efficiency that increased by nearly 85% compared with the immunoaffinity column method in the Chinese Pharmacopoeia. This established method was rapid，accurate，and highly versatile，which is suitable for the batch determination of four aflatoxins in various CMMs.

关键词

全自动免疫磁珠快速测定中药材黄曲霉毒素高效液相色谱

Keywords

automated immunomagnetic beadsrapid determinationChinese medicinal materials（CMM）aflatoxinshigh performance liquid chromatography（HPLC）

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