升麻与硫磺熏蒸升麻的FTIR法快速鉴别和区分蔡皓1,2*，赵莹莹1,2 ，刘晓1,2 ，娄雅静1,3，裴科1,2，宋晓庆1,2，乔凤仙1,2
（1.南京中医药大学药学院，江苏南京210023；2.南京中医药大学国家教育部中药炮制规范化及标准化工程研究中心，江苏南京210023；3. 江苏正大丰海制药有限公司药物研究所，江苏南京210046）
[摘要] 目的：利用傅里叶变换红外（FTIR）光谱法对升麻与硫磺熏蒸升麻进行快速鉴别。方法：采用FTIR
并结合二阶导数对升麻与硫磺熏蒸升麻的醇提物和水提物进行对比分析。结果：红外光谱显示升麻与硫磺
熏蒸升麻的醇提物和水提物在红外吸收峰峰位与相对强度上均存在差异；通过二阶导数光谱的分析，其差失落非主流
异性更加明显。在水提物的红外光谱中，硫磺熏蒸后升麻中有新的吸收峰出现，部分原有吸收峰消失；在
醇提物的红外光谱中，硫磺熏蒸后升麻产生较多新的吸收峰，吸收峰强度明显下降。二阶导数光谱显示，
在水提物中，二者在3950 cm-1 - 3940 cm-1，3850 cm-1 - 3800 cm-1，1800 cm-1 - 1750 cm-1以及1400 cm-1 - 1350
cm-1区域内有明显的变化；在醇提物中，二者在3980 cm-1 - 3960 cm-1，3850 cm-1 - 3800 cm-1以及1500 cm-1
- 1460 cm-1区域内有明显的变化。结论：FTIR和二阶导数光谱相结合可快速准确地分析和鉴别升麻与硫磺
熏蒸升麻，该方法简单并且特征性强，可为中药的质量控制提供一种有效的方法和手段。
[关键词] 升麻；硫磺熏蒸；红外光谱；二阶导数；快速鉴别和区分
Quick identification and discrimination of sun-dried and sulfur-fumigated Cimicifugae Rhizoma by Fourier transform infrared spectroscopy CAI Hao1,2*, ZHAO Ying-ying1,2, LIU Xiao1,2,LOU Ya-jing1,3, PEI Ke1,2, SONG Xiao-qing1,2,
QIAO Feng-xian1,2
(1. College of Pharmacy, Nanjing University of Chinese Medicine, Nanjing 210023, China; 2. Engin
剪刀手爱德华好看吗eering Center of State Ministry of Education for Standardization of Chinese Medicine Processing, Nanjing University of Chinese Medicine, Nanjing 210023, China; 3. Pharmaceutical Research Institute, Jiangsu Chia Tai Fenghai Pharmaceutical Co., Ltd., Nanjing 210046, China)
给市长的一封信[Abstract] Objective:To develop a method for quick identification of sun-dried and sulfur-fumigated Cimicifugae Rhizoma by Fourier transform infrared spectroscopy (FTIR). Methods: The alcoholic and aqueous extracts of sun-dried and sulfur-fumigated Cimicifugae Rhizoma were analyzed and compared by using FTIR combined with second derivative infrared spectroscopy. Results: FTIR spectra showed that there were some differences in the positions of infrared absorption peaks and the relative intensities in the alcoholic and aqueous extracts of sun-dried and sulfur-fumigated Cimicifugae Rhizoma, and the second derivative IR spectra clearly enhanced the spectral resolution of their differences. FTIR spectra showed that the new absorption peaks of Cimicifugae Rhizoma appeared and a part of original absorption peaks
disappeared after sulfur-fumigation in aqueous extracts, while a lot of new absorption peaks 基金项目：国家自然科学基金项目（81173546、30940093）；江苏省自然科学基金项目（BK2009495）；江苏省国际科技合作计划项目（BZ2011053）；国家药典委员会项目；江苏省企业博士集聚计划；江苏高校优势学科建设工程项目（2011ZYX2-001）；江苏省普通高校研究生科研创新计划项目（KYLX
_0975）
produced and the intensities of almost all absorption peaks significantly decreased after sulfur-fumigation in alcoholic extracts. Second derivative IR spectra showed that both sun-dried and sulfur-fumigated Cimicifugae Rhizoma extracted by water differed significantly from each other ranging from about 3950 cm-1 to 3940 cm-1, 3850 cm-1 to 3800 cm-1, 1800 cm-1 to 1750 cm-1, as well as from 1400 cm-1 to 1350 cm-1; differences also existed between sun-dried and sulfur-fumigated Cimicifugae Rhizoma extracted by ethanol ranging from about 3980 cm-1 to 3960 cm-1, 3850 cm-1 to 3800 cm-1, and 1500 cm-1 to 1460 cm-1. Conclusion: The FTIR method combined with the second derivative IR spectrum can be used to analyze and distinguish sun-dried and sulfur-fumigated Cimicifugae Rhizoma quickly and accurately. The developed method provides an efficient approach for the quality control of Chinese herbal medicines with its simplicity and strong specificity.
[Keywords] Cimicifugae Rhizoma; Sulfur-fumigation; Fourier transform infrared spectroscopy; Second derivative; Quick identification and discrimination
升麻为毛茛科植物大三叶升麻Cimicifuga heracleifolia Kom.、兴安升麻Cimicifuga dahurica (Turcz.)Maxim.或升麻Cimicifuga foetida L.的干燥根茎。味辛、微甘，微寒，归肺、脾、胃、大肠经。
具有发表透疹，清热解毒，升举阳气的功效[1]。近年来，为达到药材的防腐和增目的，在生产加工时多采用硫磺熏蒸的方法来干燥药材，致使药材中残留大量的二氧化硫及有害重金属，严重危害人体健康且使药材的疗效及质量大大降低[2-3]。升麻作为一味常用中药，其在市场上硫磺熏蒸的现象较为普遍，这使得相当一部分升麻药材的质量下降，因此建立快速有效的针对硫磺熏蒸加工升麻的鉴别方法势在必行。
近年来，傅里叶变换红外光谱与二阶导数谱相结合技术已逐渐被广泛应用于中药的质量控制[4-11]。本文首次将该技术应用于升麻与硫磺熏蒸升麻的快速无损鉴别研究，为升麻与硫磺熏蒸升麻的鉴别提供了一种简便迅速、直观有效的检测方法。
1实验部分制订和制定
1.1 仪器设备和参数设置
所用分析仪器为美国Nicolet IR100型傅里叶变换红外光谱仪，光谱范围4000 cm-1 – 400 cm-1，分辨率4 cm-1，扫描累加次数16次，扫描时扣除H2O和CO2的干扰。
1.2 样品来源与制备
辽中南工业基地从升麻主产地及各大药房共收集升麻药材及饮片13批，经酸蒸馏碘滴定法(GB/T 5009.34)检测，其中7
批为非硫磺熏蒸升麻，6批为硫磺熏蒸升麻；另取其中的1批非硫磺熏蒸升麻经实验室自熏作为对照（具体的产地及来源信息详见表1），上述各批次升麻经南京中医药大学药学院陈建伟教授鉴定，均为毛茛科植物大三叶升麻Cimicifuga heracleifolia Kom.的干燥根茎。
供试样醇提物的制备：称取不同批次的升麻粉末(过45目筛)各5 g，置100 mL三角烧
而硫熏升麻的吸收峰消失，也可作为二者的重要鉴别依据。
图1 硫磺熏蒸升麻样品（1-7）水提物的傅里叶变换红外光谱图
西餐菜谱图2 非硫磺熏蒸升麻样品（8-14）水提物的傅里叶变换红外光谱图
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