蝉蜕质量标准提升研究
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摘要
目的:建立并完善蝉蜕质量标准。方法:参照2015年版《中华人民共和国药典》相关方法对12批蝉蜕进行性状、显微和薄层鉴别研究,并分别测定了水分、总灰分、酸不溶性灰分、黄曲霉毒素、重金属及有害元素和浸出物的含量,通过高效液相色谱法测定4种核苷成分含量,建立蝉蜕水溶性成分HPLC指纹图谱。结果:不同批次蝉蜕的性状和显微特征较一致;氨基酸薄层色谱斑点清晰,分离度良好;水分含量为6.99%～11.44%;总灰分为17.98%～28.88%,酸不溶性灰分为13.57%～26.95%;浸出物含量为4.57%～10.59%;铅、镉、砷、铬和汞含量分别为1.730～10.300 mg/kg、0.050～1.300 mg/kg、1.200～5.700 mg/kg、5.200～17.300 mg/kg、0.007～0.115 mg/kg;蝉蜕样品均未检出黄曲霉毒素;4种核苷成分含量低且差异大,暂不纳入质量标准。12批蝉蜕样品的高效液相色谱指纹图谱相似度均大于0.900。结论:本研究所建立的方法操作简单、准确度高、重现性好,可用于蝉蜕的质量控制。
Objiective: To establish and improve the quality standard of Cicada slough. Methods: According to the methods of Chinese Pharmacopoeia(2015), this paper observed the morphological, microscopic character and thin layer identification character of 12 batches of Cicada slough. Meanwhile,water content, total ash, acid-insoluble ash aflatoxin, heavy metalsand harmful elements, and extract were also determined. At the same time, the contents of 4 Nucleoside were determined by high performance liquid chromatography(HPLC) and the fingerprint of water-soluble components of Cicada slough was established.Results:The results showed that the characters and microscopic features of the cicada sloughs were consistent in different batches. The TLC spots of amino acids were clear and the resolution was good. The water content was 6.99%～11.44%. The total ash was 17.98%～28.88%. The acid-insoluble ash was 13.57%～26.95% and the extract was 4.57%～10.59%. The contents of Pb, Ge, As, Cr and Hg were 1.730～10.300 mg/kg, 0.050～1.300 mg/kg, 1.200～5.700 mg/kg, 5.200～17.300 mg/kg, 0.007～0.115 mg/kg.Aflatoxin was not detected in any of the samples. Due to the low contents of the four nucleosides and the differences were large, they were not included in the quality standards.The similarity of HPLC fingerprints of 12 batches of Cicada slough was higher than 0.900. Conclusion:The method established in this paper can be usedfor the quality control of cicadas.
Objiective: To establish and improve the quality standard of Cicada slough. Methods: According to the methods of Chinese Pharmacopoeia(2015), this paper observed the morphological, microscopic character and thin layer identification character of 12 batches of Cicada slough. Meanwhile,water content, total ash, acid-insoluble ash aflatoxin, heavy metalsand harmful elements, and extract were also determined. At the same time, the contents of 4 Nucleoside were determined by high performance liquid chromatography(HPLC) and the fingerprint of water-soluble components of Cicada slough was established.Results:The results showed that the characters and microscopic features of the cicada sloughs were consistent in different batches. The TLC spots of amino acids were clear and the resolution was good. The water content was 6.99%～11.44%. The total ash was 17.98%～28.88%. The acid-insoluble ash was 13.57%～26.95% and the extract was 4.57%～10.59%. The contents of Pb, Ge, As, Cr and Hg were 1.730～10.300 mg/kg, 0.050～1.300 mg/kg, 1.200～5.700 mg/kg, 5.200～17.300 mg/kg, 0.007～0.115 mg/kg.Aflatoxin was not detected in any of the samples. Due to the low contents of the four nucleosides and the differences were large, they were not included in the quality standards.The similarity of HPLC fingerprints of 12 batches of Cicada slough was higher than 0.900. Conclusion:The method established in this paper can be usedfor the quality control of cicadas.
引文
[1] 国家药典委员会.中华人民共和国药典[S].北京:中国医药科技出版社,2015:369.
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[9] 邱峰,刘立行,马蔷.非完全消化-火焰原子吸收法测定蛇蜕及蝉蜕中微量元素[J].沈阳药科大学学报,2005,22(2):115-117.
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[12] 安磊.蝉蜕的抗惊厥作用[J].中国医药导报,2008,5(15):35-36.
[13] SUN Q,LI XJ,GONG SS,et al.A novel synthesis of antiviral nucleoside phosphoramidate and thiophosphoramidate prodrugs via nucleoside H-phosphonamidates [J].Nucleosides Nucleotides Nucleic Acids,2013,32(11):617.
[14] 王冬梅,刘景汉,周俊,等.腺苷对血小板体外激活的抑制作用[J].中国实验血液学杂志,2005,13(6):1094-1098.
[15] 王朋展,相美容,李灿,等.HPLC法同时测定不同来源半夏及其伪品中9种核苷类成分的含量[J].药物分析杂志,2017,37(2):212-218.
[16] Lu GH,Chan K,Liang YZ,et al.Development of high-performance liquid chromatographic fingerprints for distinguishing Chinese Angelica from related umbelliferae herbs [J].J Chromatogr A,2005,1073(2):383-392.
[17] 李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药,2013,44(22):3095-3104.
[18] 张永文.浅谈中药新药质量标准制定的整体思路[J].中国新药杂志,2017,26(18):2185-2189.
[19] 刘丽娜,李耀磊,金红宇,等.免疫亲和净化HPLC柱后光化学衍生荧光法测定动物药中黄曲霉毒素[J].中草药,2017,48(6):1220-1224.
[20] 张勇,卓宝松,刘宝岩,等.HPLC法同时测定人工蛹虫草不同部位中5种核苷类成分的含量[J].中国药房,2017,28(9):1254-1256.
[21] 岳媛,杨晓阳,肖佳佳,等.ICP-MS法测定川明参中6种重金属元素[J].中草药,2016,47(9):1595-1600.
[2] 陈蔚文.中药学[M].2版.北京:人民卫生出版社,2012:54.
[3] 李喜香,刘效栓.实用中药性状鉴别入门[M].北京:中医古籍出版社,2015:261.
[4] 高长久,张梦琪,曹静,等.蝉蜕的药理作用及临床应用研究进展[J].中医药学报,2015,43(2):110-112.
[5] 张驰,杨届.蝉蜕的药理作用及临床应用研究进展[J].湖南中医杂志,2014,30(11):194-195.
[6] 李兰铮.蝉蜕清心汤治疗小儿夜啼46例[J].实用医学杂志,2000,16(1):75.
[7] 杨明,郭丽.蚕蝉颗粒治疗儿童上气道咳嗽综合征45例临床观察[J].河北中医,2013,35(11):1640-1641.
[8] 李辉容,贾芳.蝉蜕中微量元素Ca、Fe、Zn、Mn、Cu、Cd的测定[J].绵阳师范学院学报,2008,27(11):55-58.
[9] 邱峰,刘立行,马蔷.非完全消化-火焰原子吸收法测定蛇蜕及蝉蜕中微量元素[J].沈阳药科大学学报,2005,22(2):115-117.
[10] 肖垒,袁鑫,汪华锋,等.浙江天目山地区蝉蜕微量元素含量测定及分析[J].浙江中医药大学学报,2015,39(5):378-390.
[11] 杨璐,李国玉,王金辉.蝉蜕化学成分和药理作用的研究现状[J].农垦医学,2011,33(2):184-186.
[12] 安磊.蝉蜕的抗惊厥作用[J].中国医药导报,2008,5(15):35-36.
[13] SUN Q,LI XJ,GONG SS,et al.A novel synthesis of antiviral nucleoside phosphoramidate and thiophosphoramidate prodrugs via nucleoside H-phosphonamidates [J].Nucleosides Nucleotides Nucleic Acids,2013,32(11):617.
[14] 王冬梅,刘景汉,周俊,等.腺苷对血小板体外激活的抑制作用[J].中国实验血液学杂志,2005,13(6):1094-1098.
[15] 王朋展,相美容,李灿,等.HPLC法同时测定不同来源半夏及其伪品中9种核苷类成分的含量[J].药物分析杂志,2017,37(2):212-218.
[16] Lu GH,Chan K,Liang YZ,et al.Development of high-performance liquid chromatographic fingerprints for distinguishing Chinese Angelica from related umbelliferae herbs [J].J Chromatogr A,2005,1073(2):383-392.
[17] 李强,杜思邈,张忠亮,等.中药指纹图谱技术进展及未来发展方向展望[J].中草药,2013,44(22):3095-3104.
[18] 张永文.浅谈中药新药质量标准制定的整体思路[J].中国新药杂志,2017,26(18):2185-2189.
[19] 刘丽娜,李耀磊,金红宇,等.免疫亲和净化HPLC柱后光化学衍生荧光法测定动物药中黄曲霉毒素[J].中草药,2017,48(6):1220-1224.
[20] 张勇,卓宝松,刘宝岩,等.HPLC法同时测定人工蛹虫草不同部位中5种核苷类成分的含量[J].中国药房,2017,28(9):1254-1256.
[21] 岳媛,杨晓阳,肖佳佳,等.ICP-MS法测定川明参中6种重金属元素[J].中草药,2016,47(9):1595-1600.