薄荷及其饮片中掺有易混品留兰香检测方法的实验研究

目的:从药材市场调研和国家药品评价抽验“逍遥丸”薄荷药材考察中发现,薄荷有以留兰香代用或混用的问题。两者虽为同科同属植物,但其主要成分、功能主治等存在差异。薄荷、留兰香的性状、显微相近,易发生掺伪、掺杂问题。故有必要建立能够区分薄荷和留兰香的专属性强的TLC、GC、GC-MS补充检验方法。方法:根据薄荷含薄荷脑,不含香芹酮,而留兰香含有香芹酮的特性,以薄荷脑及香芹酮为指标,建立了TLC、GC的薄荷脑的鉴别及香芹酮限量检查方法,并使用GC-MS进行确证。TLC及GC中香芹酮的限量是根据中国药典规定药材允许的杂质量、留兰香中香芹酮的平均含量及本实验方法计算而定。若超过规定限量,则用GC-MS进行确证。结果:TLC、GC方法专属性、重复性、耐用性均好,能同时鉴别薄荷中并检查留兰香中香芹酮。在企业提供及药材市场收集的23份薄荷药材中,其中5份为含有香芹酮的阳性样品,且超过规定限量,留兰香混入薄荷的比例为21.7%。有必要建立补充检验方法以鉴别、检查薄荷药材。结论:建立的方法能够检测香芹酮,解决现行标准专属性较差的问题,可有效地控制薄荷及其饮片的质量。

Objective:The problem of adulteration of Herba Menthae Spicatae in Herba Menthae was found in the herbal medicine market and also in Xiaoyao pills.The main components and functions are different between the two kinds of plants,although they belong to the same family and genus.It is difficult to find the adulteration since their characteristics are similar in appearance, microscopic and TLC.It is meaningful to find out the highly specific additional testing methods of TLC,GC and GC-MS to distinguish Herba Menthae from Herba Menthae Spicatae.Methods:The methods of TLC and GC were established with menthol and carvone as the indicators that Menthol was in Herba Menthae and carvone was in Herba Menthae Spicatae but not in Herba Menthae.The limit of carvone was set in the Herba Menthae.The limit of carvone was determined according to the limit of impurity in Chinese pharmacopoeia and the average content of carvone in Herba Menthae Spicatae.The TLC spot size and the GC chromatographic peak area should not exceed the size and area of carvone standard of 50 μg·mL^-1 if carvone was detected in the sample.Once it is in excess of the prescribed limit, the sample will be identified by GC-MS.Results:The method had good specificity,repeatability and durability.The method could identify Herba Menthae and check carvone in Herba Menthae Spicatae at the same time.The results show that carvone could be detected in 5 of the total 23 samples which come from the herbal medicine market and some pharmaceutical enterprises.The ratio was 21.7%.It was necessary to establish the test method of supplement for distinguishing Herba Menthae from Herba Menthae Spicatae.Conclusion:The established method is able to detect carvone, which is applicable to improve the quality control of Herba Menthae effectively.

[1] ChP 2010.Vol Ⅰ(中国药典2010年版.一部)[S].2010:354,395
[2] The Quality Standard of Traditional Chinese Medicinal Materials and National Medicine in Guizhou Province(贵州省中药材、民族药材质量标准)[S].2003:311
[3] CUI YH(崔宇宏),GAO TA(高天爱),AN ZQ(安志强).Distinguish Herba Menthae from Herba Menthae Spicatae(薄荷及其伪品留兰香的鉴别)[J].Guangming J Chin Med(光明中医),2011,26(8):1712
[4] FANG HL(房海灵),LI WL(李维林),LIANG CY(梁呈元),et al.Numerical classification of Mentita L.(薄荷属植物的数量分类)[J].J Anhui Agric Sci(安徽农业科学),2007,35(26):8181
[5] XIA L(夏莲).A review on the research and development of mint class resources(薄荷属资源的研究与开发利用概况)[J].Clin J Chin Med(中医临床研究), 2010,18(2):118
[6] LIANG CY(梁呈元),LIU Y(刘艳),LI WL(李维林).Plants of the genus mint external morphological diversity research(薄荷属植物外部形态多样性研究)[J].Jiangsu Agric Sci(江苏农业科学),2011,39(2):238
[7] FANG HL(房海灵),LIU Y(刘艳), LIANG CY(梁呈元),et al.Mint plant classification and breeding research overview of Mentita L.(薄荷属植物分类和育种研究概述)[J].Chin J Inf TCM(中国中医药信息杂志),2010,17(8):101
[8] FANG HL(房海灵),LI WL(李维林),REN BR(任冰如),et al.Research advance on chemical constituents and pharmacological activities of Mentha L.(薄荷属植物的化学成分及药理学研究进展)[J].China Pharm(中国药业),2010,19(10):13
[9] LI H(李宏).The quality standard and pharmaceutical applications of Mentita L.and the oil(薄荷属植物及其精油的质量标准与药学应用)[J].World Phytomed(国外医药·植物药分册),2000,15(4):146
[10] JIAN GX(剑桂新).Plants of the genus mint chemical taxonomy study and its significance(薄荷属植物化学分类学研究及其意义)[J].Chin Tradit Herb Drugs(中草药),1991,22(l1): 519
[11] GB 11960-2008 Food Additive—Standard of Spearmint Oil(食品添加剂留兰香油标准)[S]//The National Standard of the People's Republic of China(中华人民共和国国家标准).2008
[12] CAO JH(曹继华),ZHU CM(朱聪明),LI YL(李艳丽).Distinguishing Herba Menthae from Herba Menthae Spicatae(薄荷及其伪品的鉴别)[J].J Henan Univ Tradit Chin Med(河南中医学院学报),2004,19(1):110
[13] QBT 2521-2011 Standard of Spearmint Oil(留兰香(精)油标准)[S]//The Light Industry Standard of the People's Republic of China(中华人民共和国轻工业行业标准).2011