高效液相色谱法测定五氯柳胺混悬液的含量及有关物质

doi:10.3969/j.issn.1004-1524.2019.02.13

浙江农业学报 ›› 2019, Vol. 31 ›› Issue (2): 268-278.DOI: 10.3969/j.issn.1004-1524.2019.02.13

高效液相色谱法测定五氯柳胺混悬液的含量及有关物质

白玉彬¹, 张吉丽¹, 朱建民², 苏文杰², 董朕¹, 周绪正¹, 张继瑜^{1, *}

1.中国农业科学院兰州畜牧与兽药研究所,甘肃兰州 730050;
2.常州齐晖药业有限公司,江苏常州 213000

收稿日期:2018-08-13 出版日期:2019-02-25 发布日期:2019-03-06
通讯作者: 张继瑜,E-mail: infzjy@sina.com
作者简介:白玉彬(1991—),男,山东济宁人,硕士研究生,研究方向为兽医药理学与毒理学。E-mail: baiyb1011@163.com
基金资助:
国家科技支撑计划(2015BAD11B01-01); 国家肉牛牦牛产业技术体系药物开发与临床用药岗位(CARS-37)

Determination of related substances and content of oxyclozanide suspension by high performance liquid chromatography

BAI Yubin¹, ZHANG Jili¹, ZHU Jianmin², SU Wenjie², DONG Zhen¹, ZHOU Xuzheng¹, ZHANG Jiyu^{1, *}

1. Lanzhou Institute of Husbandry and Pharmaceutical Science, Chinese Academy of Agricultural Sciences, Lanzhou 730050, China;
2. Changzhou Yabang-QH Pharmachem Co., Ltd., Changzhou 213000, China

Received:2018-08-13 Online:2019-02-25 Published:2019-03-06

摘要/Abstract

摘要： 为了测定五氯柳胺混悬液的含量和有关物质,建立了一种高效液相色谱法(HPLC)。含量测定方法采用Hypersil BDS C18(150 mm×4.6 mm,5 μm)色谱柱,流动相为0.1%磷酸水-甲醇(体积比为38:62),检测波长为300 nm,柱温为25 ℃。有关物质测定方法采用InertSustainSwift C18(150 mm×4.0 mm,5 μm)色谱柱,流动相、检测波长、柱温与含量测定方法相同。结果表明,五氯柳胺混悬液检测质量浓度线性范围为34.01~104.35 μg·mL^-1(R²=1.000),平均回收率为100.1%;已知杂质2-氨基-4,6-二氯苯酚盐酸盐和3,5,6-三氯水杨酸线性范围为0.51~20.4 μg·mL^-1 (R²分别为0.996、1.000),平均回收率分别为110.3%和98.6%。本研究建立的方法方便、简单、准确,可同时测定五氯柳胺混悬液的含量及有关物质,为该产品的质量控制提供标准。

关键词: 高效液相色谱法, 五氯柳胺, 线性范围, 平均回收率

Abstract: In order to detect the content and related substances of oxyclozanide suspension, a new method using high performance liquid chromatography (HPLC) was established. Content determination was carried out using Hypersil BDS C18 (150 mm×4.6 mm, 5 μm) column and 0.1% phosphoric acid water-method (volume ratio=38:62) as mobile phase, column temperature was 25 ℃, and determination wavelength was 300 nm. Related substances was carried out using InertSustainSwift C18 (150 mm×4.0 mm,5μm) column, mobile phase, detection wavelength and column temperature were the same as the content determination method. The results showed that liner range of content determination of oxyclozanide suspension were 34.01-104.35 μg·mL^-1 (R²=1.000), and average recovery was 100.1%. The liner range of 2-amino-4, 6-dichlorophenol hydrochloride and 3, 5, 6-trichlorosalicylic acid were 0.51-20.4 μg·mL^-1 (R²=0.996, 1.000, respectively), and average recovery were 110.3% and 98.6%, respectively. It showed that the method was convenient, simple and accurate, and could simultaneously determine the content and related substances of oxyclozanide suspension, and provided standards for quality control of the product.

Key words: HPLC, oxyclozanide, linear range, the average recovery rate

中图分类号:

S859.5

白玉彬, 张吉丽, 朱建民, 苏文杰, 董朕, 周绪正, 张继瑜. 高效液相色谱法测定五氯柳胺混悬液的含量及有关物质[J]. 浙江农业学报, 2019, 31(2): 268-278.

BAI Yubin, ZHANG Jili, ZHU Jianmin, SU Wenjie, DONG Zhen, ZHOU Xuzheng, ZHANG Jiyu. Determination of related substances and content of oxyclozanide suspension by high performance liquid chromatography[J]. , 2019, 31(2): 268-278.

参考文献

[1] VEENENDAAL G H, WAAL M J D. Uncoupling activity of the anthelmintic oxyclozanide in rodents[J]. British Journal of Pharmacology, 2012, 50(3):435-437.
[2] CORBETT J R, GOOSE A J.The biochemical mode of action of the fasciolicides nitroxynil, hexachlorophane and oxyclozanide[J]. Biochemical Journal, 1971, 121(3): 41.
[3] EDWARDS S R, CAMPBELL A J, SHEERS M, et al.Studies of the effect of diamphenethide and oxyclozanide on the metabolism of Fasciola hepatica[J]. Molecular & Biochemical Parasitology, 1981, 2(5/6): 323.
[4] 蔡登棣. 五氯柳胺对家畜蠕虫的活性[J]. 中国兽医科学,1990 (11):58-61.
CAI D D.Activity of pentachloramide on livestock worms[J]. Veterinary Science in China, 1990 (11):58-61.(in Chinese)
[5] PARAUD C, GAUDIN C, PORS I, et al.Efficacy of oxyclozanide against the rumen fluke Calicophoron daubneyi in experimentally infected goats[J]. Veterinary Journal, 2009, 180(2):265-267.
[6] MOONEY L, GOOD B, HANRAHAN J P, et al.The comparative efficacy of four anthelmintics against a natural acquired Fasciola hepatica infection in hill sheep flock in the west of Ireland[J]. Veterinary Parasitology, 2009, 164(2):201-205.
[7] ATHAR L A, KHAN M N, SAJID M S, et al.Cost benefits analysis of anthelmintic treatment of cattle and buffaloes[J]. Pakistan Veterinary Journal, 2011, 31(2): 149-152.
[8] ARIAS MS, SANCHÍS J, FRANCISCO I, et al. The efficacy of four anthelmintics against Calicophoron daubneyi in naturally infected dairy cattle[J]. Veterinary Parasitology, 2013, 197(1/2): 126-129.
[9] SANABRIA R, MORENO L, ALVAREZ L, et al.Efficacy of oxyclozanide against adult Paramphistomum leydeni in naturally infected sheep[J]. Veterinary Parasitology, 2014, 206(3/4):277-281.
[10] British Pharmacopoeia Commission.British Pharmacopoeia: Veterinary[M]. British: The Stationery Office, 2013.
[11] Indian Pharmacopoeia Commission.Indian Pharmacopoeia: Volume 3[M]. Indian: National Institute of Science Communication And Information Resources, 2010: 2676-2677.
[12] 谢沐风. 如何建立高效液相色谱法测定有关物质的方法[J]. 中国医药工业杂志, 2007, 38(1):45-48.
XIE M F.How to establish a HPLC method for detemination of related substances in drugs[J]. Chinese Journal of Pharmaceuticals, 2007, 38(1):45-48. (in Chinese with English abstract)
[13] 郑金琪, 付莉娜, 刘超, 等. HPLC测定盐酸拉贝洛尔的含量及有关物质[J]. 中国现代应用药学, 2013, 30(1):86-90.
ZHENG J Q, FU L L, LIU C, et al.Determination of content and related substances of labetalol hydrochloride by HPLC[J]. Chinese Modern Applied Pharmacy, 2013, 30(1):86-90. (in Chinese with English abstract)
[14] 金鹏飞, 梁晓丽, 李琼, 等. 高效液相色谱测定盐酸决奈达隆片含量及有关物质[J]. 药物分析杂志, 2013 (3):450-453.
JIN P F, LIANG X L, LI Q, et al.HPLC determination of dronedarone hydrochloride tablets and its related substances[J]. Chinese Journal of Pharmaceutical Analysis, 2013 (3):450-453. (in Chinese with English abstract)
[15] 田红芳, 王华. HPLC-DAD法测定氟班色林原料药的含量及有关物质[J]. 中国药师, 2017 (10):1777-1780.
TIAN H F, WANG H.Determination of content and related substances of flibanserin by HPLC-DAD[J]. China Pharmacist, 2017 (10):1777-1780. (in Chinese with English abstract)
[16] 于西全, 肖华, 陈欢. 奥美拉唑肠溶胶囊的质量标准研究[J]. 中国药业, 2008, 17(22):28-29.
YU X Q, XIAO H, CHEN H.Study on quality standards of omeprazole enteric: coated capsules[J]. China Pharmaceuticals, 2008, 17(22):28-29. (in Chinese with English abstract)
[17] 周怡, 郑金琪. HPLC法测定盐酸拉贝洛尔注射液的含量和有关物质[J]. 中国药房, 2013 (9):832-834.
ZHOU Y, ZHENG J Q.Determination of content and related substances of labetalol hydrochloride injection by HPLC[J]. China Pharmacy, 2013 (9):832-834. (in Chinese with English abstract)
[18] 农业部兽药评审中心. 兽药研究技术指导原则汇编(2006—2011年)[G]. 北京: 化学工业出版社, 2012: 32-37.
[19] 中国兽药典委员会. 中国兽药典: 一部[M]. 北京: 中国农业出版社, 2015: 附录66-70.
[20] FAIRWEATHER I, BORAY J C.Fasciolicides efficacy, actions resistance and its management[J]. The Veterinary Journal, 1999, 158(2): 81-112.
[21] OVEREND D J, BOWEN F L.Resistance of Fasciola hepatica to triclabendazole[J]. Australian Veterinary Journal, 2010, 72(7):275-276.
[22] 崔莹. 驱虫药五氯柳胺的制备[J]. 现代商贸工业, 2010, 22(20):300.
CUI Y.Preparation of anthelmintic oxyclozanide[J]. Modern Business Trade Industry, 2010, 22(20):300. (in Chinese)
[23] 刘祥宜, 朱建民, 张建峰, 等. 五氯柳胺的合成[J]. 浙江化工, 2010, 41(8): 11-12.
LIU X Y, ZHU J M, ZHANG J F, et al.Synthesis of oxyclozanide[J]. Zhejiang Chemical Industry, 2010, 41(8):11-12. (in Chinese)
[24] 王学成, 苏文杰, 刘祥宜, 等. 五氯柳胺合成工艺改进[J].浙江化工, 2017, 48(5):18-19.
WANG X C, SU W J, LIU X Y, et al.Improvement of synthesis process of pentamidine[J]. Zhejiang Chemical Industry, 2017, 48(5):18-19. (in Chinese)

高效液相色谱法测定五氯柳胺混悬液的含量及有关物质

Determination of related substances and content of oxyclozanide suspension by high performance liquid chromatography

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