蜈蚣药材中3,8-二羟基喹啉的定性定量分析方法研究

目的：建立蜈蚣药材的定性定量分析方法。方法：采用薄层色谱法对蜈蚣药材进行定性鉴别，以三氯甲烷-甲醇-甲酸（10∶1∶1）为展开剂，在紫外光灯（254 nm）下检视；运用高效液相色谱法测定3，8-二羟基喹啉的含量，采用Kromasil C₁₈（250 mm×4.6 mm，5 μm）色谱柱，流动相为甲醇-10 mmol·L^-1的磷酸二氢钾溶液（32∶68），流速0.8 mL·min^-1，检测波长252 nm，柱温40℃。结果：薄层鉴别斑点清晰，分离度良好；含量测定中，3，8-二羟基喹啉的线性范围为0.036 2~0.289 6 μg（r=0.999 4），平均加样回收率为99.2%（RSD=1.4%，n=6），17批样品中3，8-二羟基喹啉的含量范围为0.175~2.28 mg·g^-1。结论：本文建立的薄层色谱鉴别及高效液相色谱含量测定方法可用于蜈蚣药材的质量控制。

Objective: To establish qualitative and quantitative methods of Scolopendra. Methods: TLC method was used for qualitative identification of Scolopendra. The plate was developed with chloroform-methanolformic acid(10:1:1) and detected under ultraviolet light at 254 nm. The content of 3, 8-dihy droxy quinolone was determined by HPLC. A Kromasil C₁₈(250 mm×4.6 mm, 5 μm) column was used, and the mobile phase was methanol-10 mmol·L^-1 potassium dihydrogen phosphate(32:68) at a flow rate of 0.8 mL·min^-1. The detection wavelength was set at 252 nm and the column temperature was 40℃. Results: TLC spots were clear and well separated. 3, 8-dihydroxy quinoline showed a good linear relationship at the range of 0.036 2-0.289 6 μg(r=0.999 4). The average recovery was 99.2%(RSD=1.4%, n=6) and the content range in seventeen batches of samples was 0.175-2.28 mg·g^-1. Conclusion: The proposed TLC identification and HPLC assay methods could be used for quality control of Scolopendra.

[1] 中国药典2015年版.一部[S]. 2015:357 ChP 2015. V ol Ⅰ[S]. 2015:357
[2] 陈武忠,曹海燕.中药蜈蚣的研究进展[J].中国现代中药, 2011, 13(7):54 CHEN WZ, CAO HY. Research progress of traditional Chinese medicine centipede[J]. Mod Chin Med,2011, 13(7):54
[3] 苗明三.现代实用中药质量控制技术[M].北京:人民卫生出版社, 2000:1055 MIAO MS. Modern Practical TCM Quality Control Technology[M]. Beijing:People's Medical Publishing House,2000:1055
[4] 王贤纯.蜈蚣的药用研究进展[J].动物学杂志,2002,37(3):88 WANG XC. A review on the medical application of centipede[J]. Chin J Zool,2002, 37(3):88
[5] 周永芹,韩莉,刘朝奇,等.蜈蚣提取物对小鼠宫颈肿瘤生长的影响及其作用机制的实验研究[J].中药材, 2011, 34(6):859 ZHOU YQ, HAN L, LIU ZQ, et al. Effects of centipede extract on cervical tumor of mice and its mechanism[J]. J Chin Med Mater, 2011, 34(6):859
[6] 姜建伟,何福根,章红燕.中药蜈蚣抗肿瘤作用机制及临床应用研究进展[J].海峡药学,2012, 24(9):28 JIANG JW, HE FG, ZHANG HY. Research progress on the antitumor mechanism and clinical application of centipede[J]. Strait Pharm J,2012, 24(9):28
[7] 王丽娜,何玲,程卉,等.蜈蚣提取液对局灶性脑缺血再灌注大鼠血浆vWF和TPO的影响[J].中国实验方剂学杂志,2012, 18(14):192 WANG LN,HE L,CHENG H,et al. Effects of centipede extraction on vWF and TPO expression in blood plasm after focal cerebral ischemia-reperfusion injury in rats[J]. Chin J Exp Tradit Med Form,2012, 18(14):192
[8] 刘瑞连,廖建萍,刘绍贵.蜈蚣不同部位抗凝活性的研究[J].中医药导报, 2015, 21(2):32 LIU RL,LIAO JP,LIU SG. Study on the anticoagulant of different extracts of centipede[J]. Guid J Tradit Chin Med Pharm,2015,21(2):32
[9] 方秀桐,莫可.蜈蚣的药理研究进展[J].中国医药指南,2015, 13(18):32 FANG XT,MO K. Advances in the study on pharmacological effects of centipede[J]. Guide Chin Med,2015, 13(18):32
[10] 刘继红,尚娟,贾斌,等.蜈蚣、全蝎、地龙氨基酸含量测定[J]. 郑州大学学报(医学版), 2005, 40(3):483 LIU JH, SHANG J, JIA B, et al. Detection of amino acid in centipede, whole scorpion, and earth worm[J]. J Zhengzhou Univ Med Sci,2005, 40(3):483
[11] 方红,邓芳.蜈蚣药材中毒性成分组织胺的含量测定[J].中草药, 1997, 28(8):472 FANG H,DENG F. Determination of the contents of histamine in the toxic components of centipede[J]. Chin Tradit Herb Drugs,1997,28(8):472
[12] 刘丽芳,金蓉鸾,徐国钧. HPLC法测定10种动物药中尿嘧啶、黄嘌呤、次黄嘌呤、脲苷的含量[J].中国中药杂志,1999,24(2):73 LIU LF, JIN RL, XU GJ. HPLC determination of uracil, xanthine, hypoxanthine and uridine in ten species of animal drugs[J]. China J Chin Mater Med,1999, 24(2):73
[13] MOON SS,CHO N,SHIN J,et al. Jineol,a cytotoxic alkaloid from the Centipede Scolopendra subspinipes[J]. J Nat Prod,1996,59(8):777
[14] 孙琳娜.蜈蚣中有效成分的研究[D].天津:天津理工大学,2015 SUN LN. Studies on the Effective Constituents of Scolopendra subspinipes[D]. Tianjin:Tianjin University of Technology,2015
[15] 朴镐用,郑泰淑,吴贤宇,等.预防和治疗心血管疾病的新型喹啉化合物,以及含有蜈蚣提取物或从提取物中分离的化合物的组合物:中国,102670571 A[P]. 2012-09-19 PARK HY, JEONG TS, OH HW, et al. Quinoline Compound, and Composition Containing Centipede Extract or Compounds Isolated Therefrom for Prevention and Treatment of Cardiovascular Disease:China, 102670571 A[P]. 2012-09-19