烯丙孕素口服液在猪体内的残留消除研究

doi:10.11843/j.issn.0366-6964.2018.09.022

畜牧兽医学报 ›› 2018, Vol. 49 ›› Issue (9): 2005-2014.doi: 10.11843/j.issn.0366-6964.2018.09.022

烯丙孕素口服液在猪体内的残留消除研究

王双^1,2, 杨海峰^1,2, 余波^1,3, 李士洋^1,3, 郑育基^1,3, 卜仕金^1,3*

1. 扬州大学兽医学院, 扬州 225009;
2. 江苏农牧科技职业学院, 泰州 225300;
3. 江苏省动物重要疫病与人畜共患病防控协同创新中心, 扬州 225009

收稿日期:2018-01-17 出版日期:2018-09-23 发布日期:2018-09-23
通讯作者: 卜仕金(1964-),男,安徽人,教授,主要从事兽医药理与毒理学研究,E-mail:pushijin@aliyun.com
作者简介:王双(1993-),女,河南人,硕士生,主要从事药理学研究,E-mail:1289656619@qq.com
基金资助:
江苏省普通高校研究生科研创新计划项目（SJLX15＿0675）；扬州大学“新世纪人才工程”资助项目

Study on Residue Elimination of Altrenogest Oral Solution in Pigs

WANG Shuang^1,2, YANG Hai-feng^1,2, YU Bo^1,3, LI Shi-yang^1,3, ZHENG Yu-ji^1,3, BU Shi-jin^1,3*

1. College of Veterinary Medicine, Yangzhou University, Yangzhou 225009, China;
2. Jiangsu Agri-animal Husbandry Vocational College, Taizhou 225300, China;
3. Jiangsu Co-innovation Center for Prevention and Control of Important Animal Infections Diseases and Zoonoses, Yangzhou 225009, China

Received:2018-01-17 Online:2018-09-23 Published:2018-09-23

摘要/Abstract

摘要：

本研究旨在分析烯丙孕素在猪体内的残留消除规律，为制定休药期提供依据。采集猪肝、肾、肌肉和脂肪样品，肝、肾样品经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解，然后用乙腈提取（肌肉和脂肪样品直接用乙腈提取），乙腈饱和正己烷溶液除脂，氮吹后残渣用乙酸乙酯复溶，后用10%碳酸钠溶液净化进行LC-MS/MS分析，外标法定量。结果表明：在1~200 ng·mL^-1浓度范围内，烯丙孕素具有良好的线性关系，相关系数大于0.999，方法的检测限为0.5 μg·kg^-1，定量限为1 μg·kg^-1；在1、100、200 μg·kg^-1添加水平下，化合物的平均回收率在68.9%~78.9%，相对标准偏差均小于11%。试验猪按0.4 mg·kg^-1剂量内服给药，每天1次，连续给药18 d，经取材检测，休药6 h后各组织中烯丙孕素残留量最高，休药后第5天脂肪中烯丙孕素残留量低于最大残留限量，肌肉、肾中残留量低于定量限，休药第10天所有组织中烯丙孕素残留量均低于定量限。休药后相同时间点猪组织中烯丙孕素残留量规律为肝 > 肾 > 脂肪 > 肌肉；肝中烯丙孕素消除缓慢且消除时间最长。根据WT1.4软件按99%置信区间计算所得，建议母猪按0.4 mg·kg^-1剂量内服给药，每天1次，连续18 d，其休药期为9 d。

Abstract:

The experiment was conducted to study the residues of altrenogest in swine tissues, preparing for the determination of withdrawal time. The liver and kidney samples were hydrolyzed by β-glucosidase/arysulfatase and extracted by acetonitrile (the muscle and fat samples were extracted by acetonitrile), then the extracting solution were degreased with n-hexane. After being redissolved with ethyl acetate, the supernatant was purified by 10% sodium carbonate solution. Finally, altrenogest was analyzed by LC-MS/MS, and was calibrated by the external method. The results showed that the standard curve was obtained with the correlation coefficients (R²=0.999) in the concentration range of 1-200 ng·mL^-1. The limit of quantification for altrenogest was 1.0 μg·kg^-1, and the limit of detection for altrenogest was 0.5 μg·kg^-1. The recoveries of altrenogest were 68.9%-78.9% at three spiked levels of 1, 100, 200 μg·kg^-1 with the relative standard deviations less than 11% (n=6). After the pigs were orally administered altrenogest of 0.4 mg·kg^-1 of body weight onetime every day for 18 d, the concentration of in all of the tissues at 6 h was highest; the concentration of altrenogest in fat at 5 d was lower than MRL, while the concentration of altrenogest in muscle and kidney tissues were lower than LOQ; the concentration of altrenogest in all of the tissues at 10 d were lower than LOQ. The order of residue rate was liver > kidney > fat > muscle, and liver was considered as the target organ. The concentration-time dates were analyzed by WT1.4 to get the withdrawal time with 99% upper tolerance limit, the WT advised was 9 d.

中图分类号:

S859.84

王双, 杨海峰, 余波, 李士洋, 郑育基, 卜仕金. 烯丙孕素口服液在猪体内的残留消除研究[J]. 畜牧兽医学报, 2018, 49(9): 2005-2014.

WANG Shuang, YANG Hai-feng, YU Bo, LI Shi-yang, ZHENG Yu-ji, BU Shi-jin. Study on Residue Elimination of Altrenogest Oral Solution in Pigs[J]. ACTA VETERINARIA ET ZOOTECHNICA SINICA, 2018, 49(9): 2005-2014.

0
/ / 推荐

导出引用管理器 EndNote|Reference Manager|ProCite|BibTeX|RefWorks

链接本文: https://www.xmsyxb.com/CN/10.11843/j.issn.0366-6964.2018.09.022

https://www.xmsyxb.com/CN/Y2018/V49/I9/2005

参考文献

[1] VAN LEEUWEN J J J, MARTENS M R T M, JOURQUIN J, et al. Variation in LH pulsatility during 24 h after a postweaning altrenogest treatment in relation to follicle development in primiparous sows[J]. Anim Reprod Sci, 2011, 126(1-2):101-107.
[2] HODGSON D, HOWE S, JEFFCOTT L, et al. Effect of prolonged use of altrenogest on behaviour in mares[J]. Vet J, 2005, 169(1):113-115.
[3] VANDERHAEGHE C. 烯丙孕素对母猪早产和繁殖性能的影响[J]. 志强, 译. 中国畜牧业, 2012(12):66.
VANDERHAEGHE C. Effects of altrenogest on premature delivery and reproductive performance of sows[J]. Zhiqiang, translate. China Animal Industry, 2012(12):66. (in Chinese)
[4] WILLMANN C, SCHULER G, HOFFMANN B. Effects of age and altrenogest treatment on conceptus development and secretion of LH, progesterone and eCG in early-pregnant mares[J]. Theriogenology, 2011, 75(3):421-428.
[5] 康海宁, 谢丽琪, 肖来龙, 等. 超高效液相色谱-串联质谱法对河豚鱼、鳗鱼及烤鳗中烯丙孕素与氯地孕酮残留的同时测定[J]. 分析测试学报, 2009, 28(10):1180-1184.
KANG H N, XIE L Q, XIAO L L, et al.Determination of altrenogest and chlormadinone residues in swellfish, eel, roasted eel by ultra performance liquid chromatography-tandem mass spectrometry[J]. Journal of Instrumental Analysis, 2009, 28(10):1180-1184. (in Chinese)
[6] ZHANG D, PARK J A, KIM S K, et al. Determination of residual levels of naloxone, yohimbine, thiophanate, and altrenogest in porcine muscle using QuEChERS with liquid chromatography and triple quadrupole mass spectrometry[J]. J Sep Sci, 2016, 39(5):835-841.
[7] WAMMER K H, ANDERSON K C, ERICKSON P R, et al. Environmental photochemistry of altrenogest:Photoisomerization to a bioactive product with increased environmental persistence via reversible photohydration[J]. Environ Sci Technol, 2016, 50(14):7480-7488.
[8] KENYON P. Analytical methods for the detection and quantification of trenbolone acetate metabolites, altrenogest and related photoproducts via liquid chromatography tandem mass spectrometry[D]. Washington:University of Washington, 2015.
[9] 中华人民共和国国家质量监督检验检疫总局. SN/T 1980-2007 进出口动物源性食品中孕激素类药物残留量的检测方法高效液相色谱-质谱/质谱法[S]. 北京:中国标准出版社, 2007.
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China. SN/T 1980-2007 Determination of progestogens residues in food of animal origin for import and export-HPLC-MS/MS method[S]. Beijing:Standards Press of China, 2007. (in Chinese)
[10] EMEA. Committee for veterinary medicinal products:Altrenogest summary report(2)[R]. EMEA/MRL/831/01-FINAL, London:EMEA, 2002.
[11] MORGAN S, MACKAY A. Summary of product characteristics[M]//STOLERMAN I P. Encyclopedia of Psychopharmacology. Berlin, Heidelberg:Springer, 2010.
[12] LAMPINEN-SALOMONSSON M, BECKMAN E, BONDESSON U. Detection of altrenogest and its metabolites in post administration horse urine using liquid chromatography tandem mass spectrometry-increased sensitivity by chemical derivatisation of the glucuronic acid conjugate[J]. J Chromatogr B, 2006, 833(2):245-256.
[13] JANSEN E H J M, ZOONTJES P W, BOTH-MIEDEMA R, et al. Screening of parts-per-billion levels of diethylstilbestrol in bovine urine by high-performance liquid chromatography with ultraviolet detection[J]. J Chromatogr A, 1985, 347:379-383.
[14] ZIECIK A J, KLOS J, PRZYGRODZKA E, et al. Aberrant effects of altrenogest and exposure to exogenous gonadotropins on follicular cysts appearance in gilts[J]. Theriogenology, 2017, 89:250-254.
[15] EMEA. Committee for veterinary medicinal products:Altrenogest summary report[R]. EMEA/MRL/487/477, London:EMEA, 2012.
[16] Freedom of information summary original abbreviated new animal drug application[R]. ANADA, 2017:200-621.

烯丙孕素口服液在猪体内的残留消除研究

Study on Residue Elimination of Altrenogest Oral Solution in Pigs

RichHTML

PDF

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 11

编辑推荐

Metrics

本文评价

[1]	黄婧洁, 李苗, 陈莹娴, 钟雅兰, 张婷婷, 姜廷超男, 李建成. 基于免疫磁珠净化间接竞争酶联免疫吸附试验检测氟喹诺酮类药物[J]. 畜牧兽医学报, 2023, 54(2): 766-778.
[2]	王子琳, 唐子恒, 林泽宁, 刘文字, 刘戎, 张嘉慧, 沈祥广. 中药成分辛弗林对胶体金免疫层析法检测β-受体激动剂的影响[J]. 畜牧兽医学报, 2021, 52(12): 3675-3680.
[3]	陈莹娴, 马月姣, 李建成. 抗球虫药物残留的免疫检测技术[J]. 畜牧兽医学报, 2021, 52(4): 899-908.
[4]	曹玉颖, 王杰, 张希墨, 吴琴尧, 邱基程, 李淑媛, 张璐, 龚晓会, 白如念, 曹兴元. 盐酸多西环素片在羔羊体内残留消除规律及休药期分析[J]. 畜牧兽医学报, 2021, 52(4): 1086-1093.
[5]	张静，周倩，唐梦君，张小燕，赵敏，杨星星，万玉，高玉时. 疫苗油佐剂在鸡蛋和组织中的残留代谢分析[J]. 畜牧兽医学报, 2017, 48(3): 544-551.
[6]	高金芳,岳婷婷，赵祎,陈冬梅,袁宗辉. 兽药多残留样品前处理技术研究进展[J]. 畜牧兽医学报, 2017, 48(1): 8-22.
[7]	孙礼瑞，谢星，谢恺舟，张小杰，王剑锋，崔璐璐，刘建宇，张跟喜，戴国俊，王金玉. 氨苄西林在鸡组织中的残留消除规律[J]. 畜牧兽医学报, 2015, 46(1): 130-137.
[8]	李帅鹏，黄显会，孔祥凯，怀彬彬，王伟，王辉. 肌注马波沙星在猪组织中残留消除规律[J]. 畜牧兽医学报, 2014, 45(5): 827-832.
[9]	程古月，彭娟，王玉莲，董小冰，彭大鹏，郝海红，黄玲利，袁宗辉. β-内酰胺类抗生素残留受体分析法的研究进展[J]. 畜牧兽医学报, 2014, 45(3): 354-362.
[10]	李帅鹏，黄显会，孔祥凯，张晓会，李向阳. 头孢噻呋在猪组织中残留消除规律[J]. 畜牧兽医学报, 2013, 44(8): 1311-1316.
[11]	姜金庆，杨雪峰，王自良，邓瑞广，王选年，张改平. 克伦特罗和莱克多巴胺多残留胶体金免疫层析试纸条的研制[J]. 畜牧兽医学报, 2013, 44(1): 87-94.