商品中药材蒲黄的真伪优劣鉴别研究

目的:为商品中药材蒲黄的真伪鉴别及质量优劣评价提供依据。方法:收集我国9个不同地区生产的蒲黄药材,从外观、颜色、触感、气味、水试等方面比较受试药材与对照药材的性状特征差异;采用明场正常光与暗场偏振光对比观察各批次药材的显微特征,利用实时景深拓展技术进行拍摄以获取清晰的显微影像;以异鼠李素-3-O-新橙皮苷和香蒲新苷为对照品,对受试药材和对照药材进行薄层色谱鉴别,并结合薄层色谱-质谱联用技术鉴定可能的掺杂物。结果:9个批次的商品蒲黄药材中仅有44%符合《药典》标准,22%有掺杂品或染色,33%为纯伪品。其中,编号2、3、7、10的受试药材性状特征及显微特征与对照药材相符,薄层色谱中与对照药材和对照品在相应位置显相同颜色的荧光斑点,可鉴定为蒲黄正品;编号5的受试药材颜色和触感均与对照药材不符,显微鉴别显示大量纤维、晶体等非药用部位,推测为掺伪蒲黄;编号9的受试药材在色谱鉴别中检出染料金胺O斑点,推测为染色蒲黄;编号4、6、8的受试药材性状鉴别、显微鉴别、薄层色谱鉴别的结果均与《药典》标准不符,且质谱鉴定含有染料金胺O,故为纯伪品。结论:市售的商品蒲黄药材掺伪、造假及染色情况严重。偏振光显微影像拍摄技术、高效薄层色谱技术及薄层色谱-质谱联用技术的综合应用能够快速、高效地实现蒲黄药材的真伪鉴别及质量评价。

Identification research on authenticity and quality of commercial Typhae Pollen

  Objective:To provide the basis for authenticity identification and quality evaluation of commercial Typhae Pollen.   Methods:Typhae Pollen medicinal materials produced in nine different areas of China were collected, and the shape and property characteristics differences of tested and control medicinal materials were compared in terms of appearance, color, touch, odor and water test. The microscopic characteristics of each batch of medicinal materials were observed by the normal light of bright field and polarized light of dark field, and real-time depth of field expansion technique was used to obtain clear microscopic images. Taken isorhamnetin 3-O-neohesperidoside and typhaneoside as standards, the thin layer chromatography (TLC) was conducted to identify the tested and control medicinal materials, which combined with thin layer chromatography-mass spectrometry (TLC-MS) to identify the possible dopants.   Results:Among the nine batches of commercial medicinal materials of Typhae Pollen, only 44% were qualified with pharmacopoeia standards, 22% contain dopants or were dyed products, and 33% were pure counterfeits. Among them, the shape and property and microscopic characteristics of tested medicinal materials numbered 2,3, 7 and 10 were consistent with the control medicinal material, the fluorescent spots with the same color were displayed in the corresponding positions of the control medicinal material and the control substances in TLC, which could be identified as authentic Typhae Pollen. The color and touch of the tested medicinal material numbered 5 were inconsistent with the control medicinal material, and the microscopic identification showed a large number of non-medicinal parts such as fibers and crystals, which were presumed to be Typhae Pollen adulteration. In the chromatographic identification of the tested medicinal material numbered 9, the spot of dye auramine O was detected, so it was speculated to be dyed Typhae Pollen. The shape and property identification, microscopic identification and TLC identification of the tested medicinal materials numbered 4,6 and 8 were all inconsistent with the pharmacopoeia standards, and the containing auramine O was identified by mass spectrometry, which were considered to be complete counterfeit.   Conclusion:The adulteration, falsification and dyeing of commercial Typhae Pollen are serious. The integrated application of polarized light microscopy, high performance thin layer chromatography and thin layer chromatography-mass spectrometry can quickly and efficiently complete the authenticity identification and quality evaluation of Typhae Pollen.