方格星虫的质量检测方法及质量控制标准

Establishment of quality control methods and standards for Sipunculus nudus

目的:建立方格星虫干品质量检测标准,为其质量检测和科学开发利用提供参考。方法:参照2020版《中国药典》(四部)对来自3个不同产地的30批方格星虫干品进行性状、显微鉴别和薄层色谱(TLC)鉴别研究,检测活性物质氨基酸和总糖质量分数,检测其杂质、水分、总灰分、酸不溶灰分、重金属、水溶性浸出物质量分数,利用高效液相色谱法(HPLC)测定方格星虫的黄曲霉毒素质量分数。结果:方格星虫体壁似蚯蚓纵横交错成格状,显微观察可见先端淡棕色钝圆刚毛;在精氨酸、丙氨酸和甘氨酸处呈TLC特征色谱;氨基酸质量分数检测占比最高的依次为谷氨酸、精氨酸和天冬氨酸;总糖质量分数不低于2%;方格星虫供试品杂质、水分、总灰分和酸不溶灰分分别不超过3%、11%、10%和2%;水溶性浸出物质量分数不低于38%;黄曲霉毒素质量分数不超过10μg/kg。结论:本研究建立的方格星虫质量检测标准方法稳定,可为方格星虫药材质量控制提供参考。

Objective:The present study sought to establish quality control standards for dried checkered Sipunculus nudus products,providing a value reference for quality assessment and scientific development and utilization.Methods:The characteristics,microscopic identification,and thin-layer chromatography(TLC)identification of 30 batches of dry Sipunculus nudus from three different sources were studied following the guidelines of the Chinese Pharmacopoeia(2020 edition).Additionally,the content of active substances,including amino acids and total sugars,was measured.The impurities,moisture content,total ash content,acid-insoluble ash content,heavy metals,and water-soluble extract content were determined using supplementary tests.The content of aflatoxin in dry Sipunculus nudus was determined using high-performance liquid chromatography(HPLC).Results:The body wall of dry Sipunculus nudus is reminiscent of an earthworm,with a lattice-like structure that crisscrosses.Microscopic examination reveals light brown,blunt,and rounded bristles at the apex.Furthermore,thin-layer chromatography(TLC)analysis exhibits characteristic chromatographic patterns for arginine,alanine,and glycine.The analysis of amino acid content revealed that glutamic acid,arginine,and aspartic acid were the most abundant.The total sugar content was 2%,while the impurities,moisture content,total ash content,and acid-insoluble ash content of dry Sipunculus nudus were 3%,11%,10%,and 2%,respectively.Moreover,the water-soluble extract content was 38%,while the aflatoxin content in dry Sipunculus nudus was not more than 10μg/kg.Conclusion:The established quality testing methods for dry Sipunculus nudus possess great stability,providing a reference for the quality control of this medicinal material.