高效液相色谱法测定饲料中艾司唑仑的含量
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- 英文论文题名：Determination of Estazolam in feeds by High Performance Liquid Chromatography
- 论文作者：方秋华 ; 肖田安 ; 伍宏凯 ; 胡苑玲
- 英文论文作者：FANG Qiu-hua ; XIAO Tian-an ; WU Hong-kai ; HU Yuan-ling ; Guangdong Institute for Veterinary Drugs and Feedstuffs Control
- 年：2016
- 作者机构：广东省兽药饲料质量检验所;
- 论文关键词：艾司唑仑 ; 饲料 ; 高效液相色谱
- 英文论文关键词：Estazolam ; feeds ; high performance liquid chromatography(HPLC)
- 会议召开时间：2016-09-18
- 会议录名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会论文集
- 语种：中文
- 分类号：S816.17
- 学会代码：ZGXJ
- 会议名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会
- 会议地点：中国四川成都
- 主办单位：中国畜牧兽医学会动物药品学分会
- 学会名称：中国畜牧兽医学会
- 页数：6
- 文件大小：544k
- 原文格式：O
- 会议级别：全国
摘要
本研究建立了高效液相色谱法测定预混合饲料、配合饲料和浓缩饲料中艾司唑仑含量的检测方法。试样用正己烷-二氯甲烷(1:1,V/V)提取,经MCX固相萃取柱进一步净化,采用反相高效液相色谱-紫外检测法进行定量分析。饲料中艾司唑仑的检测限为0.1 mg/kg,定量限为0.25 mg/kg。在饲料中添加0.25,0.5,2.5 mg/kg水平的药物回收试验中,平均回收率均在82.8%~105.9%之间,相对标准偏差为1.62%~8.40%。该方法灵敏、准确,适用于饲料中艾司唑仑含量的分析检测。
A confirmatory method has been developed and validated for the determination of estazolam(EZL) in premix,compound feed and concentrate feed using high performance liquid chromatography(HPLC).The analyte was extracted from feeds using hexane-dichloromethane(1:1,V/V),and then the sample extracts were purified by MCX solid-phase extraction.The analyte was analyzed by HPLC-UV.The limit of detection was 0.1 mg/kg for EZL,with quantification limit of 0.25 mg/kg.Recoveries were in the range 82.8%to 105.9%from feeds fortified at the 0.25,0.5,2.5 mg/kg levels,and the mean intra-laboratory reproducibility ranged from 1.62%to 8.40%(%R.S.D).The developed method is sensitive and specific for the detection of estazolam in feeds.
A confirmatory method has been developed and validated for the determination of estazolam(EZL) in premix,compound feed and concentrate feed using high performance liquid chromatography(HPLC).The analyte was extracted from feeds using hexane-dichloromethane(1:1,V/V),and then the sample extracts were purified by MCX solid-phase extraction.The analyte was analyzed by HPLC-UV.The limit of detection was 0.1 mg/kg for EZL,with quantification limit of 0.25 mg/kg.Recoveries were in the range 82.8%to 105.9%from feeds fortified at the 0.25,0.5,2.5 mg/kg levels,and the mean intra-laboratory reproducibility ranged from 1.62%to 8.40%(%R.S.D).The developed method is sensitive and specific for the detection of estazolam in feeds.
引文
[1]中华人民共和国农业部.禁止在饲料和动物饮用水中使用的药物品种,北京:中华人民共和国农业部公告第176号,2002.
[2]郭胜才,邹晓华,张玉荣,等.高效液相色谱法同时测定血浆中艾司唑仑、三唑仑和阿普唑仑浓度[J].中国医院药学杂志,2003,23(10):599-601.
[3]熊建华,王淑君.高效液相色谱法同时测定人血清中4种苯二氮卓类药物浓度[J].海峡药学,2004,16(1):47-49.
[4]Masatomo MIURA,Tadashi OHKUBO,Kazunobu SUGAWARA,et al.Determination of Estazolam in Plasma by High-Performance Liquid Chromatography with Solid-Phase Extraction[J].ANALYTICAL SCIENCES,2002,18(5):525-528.
[5]侯大平,张志国,国玉芝,等.HPLC法测定艾司唑仑血药浓度的方法验证[J].中国药房,2011,22(14):1280-1282.
[6]刘福.高效液相色谱法测定艾司唑仑血浓度[J].中国药师,2007,10(11):1152-1153.
[7]叶美娣,滕彦,汪东海.HPLC法测定地西泮和艾司唑仑的血药浓度[J].中国现代应用药学杂志,2000,17(1):60-62.
[8]李淑芳,安荣姝,马秉智,等.RP-HPLC同时测定人体内盐酸纳洛酮和艾司唑仑血药浓度[J].中国药学杂志,2010,45(5):376-378.
[9]Toshimasa Toyo'oka,Yusuke Kumaki,Masayoshi Kanbori,et al.Determination of hypnotic benzodiazepines(alprazolam,estazolam,and midazolam)and their metabolites in rat hair and plasma by reversed-phase liquid-chromatography with electrospray ionization mass spectrometry[J].Journal of Pharmaceutical and Biomedical Analysis,2003,30(6):1773-1787.
[10]Toshimasa Toyo'oka,Masayoshi Kanbori,Yusuke Kumaki,et al.Detection of Triazolam and Its Hydroxy Metabolites in Rat Hair by Reversed-Phase Liquid Chromatography with Electrospray Ionization Mass Spectrometry[J].Journal of Analytical Toxicology,2000,24(3):194-201.
[11]孙雷,张骊,徐倩,等.超高效液相色谱-串联质谱法检测猪肉和猪肾中残留的10种镇静剂类药物[J].色谱,2010,28(1):38-42.
[12]许成保,锁然,张峰,等.超高效液相色谱-四极杆飞行时间质谱快速检测动物饲料中10种违禁精神药物[J].色谱,2012.30(5):457-462.
[13]索德成,赵根龙,李兰,等.液相色谱-串联质谱法同时检测饲料中7种精神类药物[J].分析化学研究简报,2010,38(7):1023-1026.
[14]严丽娟,张峰,吴敏,等.UPLC-ESI MS/MS法测定动物饲料中苯二氮卓类药物[J].分析测试学报,2011,30(11):1301-1305.
[15]Dennis J.Crouch,Douglas E.Rollins,Dennis V.Canfield,et al.Quantitation of Alprazolam and cz-Hydroxyalprazolam in Human Plasma Using Liquid Chromatography Electrospray Ionization MS-MS[J]Journal of Analytical Toxicology,1999,23(6):479-485.
[16]陈琴华,罗尚文,陈子林,等.HPLC-MS法同时测定5种抗癫痫药的血药浓度[J].中国科学:化学,2010,40(6):762-767.
[17]顾景凯,夏荣,钟大放,等。LC/MS~n法同时检测人尿液中艾司唑仑、阿普唑仑和三唑仑[J].药学学报,2002,37(2):138-140.
[2]郭胜才,邹晓华,张玉荣,等.高效液相色谱法同时测定血浆中艾司唑仑、三唑仑和阿普唑仑浓度[J].中国医院药学杂志,2003,23(10):599-601.
[3]熊建华,王淑君.高效液相色谱法同时测定人血清中4种苯二氮卓类药物浓度[J].海峡药学,2004,16(1):47-49.
[4]Masatomo MIURA,Tadashi OHKUBO,Kazunobu SUGAWARA,et al.Determination of Estazolam in Plasma by High-Performance Liquid Chromatography with Solid-Phase Extraction[J].ANALYTICAL SCIENCES,2002,18(5):525-528.
[5]侯大平,张志国,国玉芝,等.HPLC法测定艾司唑仑血药浓度的方法验证[J].中国药房,2011,22(14):1280-1282.
[6]刘福.高效液相色谱法测定艾司唑仑血浓度[J].中国药师,2007,10(11):1152-1153.
[7]叶美娣,滕彦,汪东海.HPLC法测定地西泮和艾司唑仑的血药浓度[J].中国现代应用药学杂志,2000,17(1):60-62.
[8]李淑芳,安荣姝,马秉智,等.RP-HPLC同时测定人体内盐酸纳洛酮和艾司唑仑血药浓度[J].中国药学杂志,2010,45(5):376-378.
[9]Toshimasa Toyo'oka,Yusuke Kumaki,Masayoshi Kanbori,et al.Determination of hypnotic benzodiazepines(alprazolam,estazolam,and midazolam)and their metabolites in rat hair and plasma by reversed-phase liquid-chromatography with electrospray ionization mass spectrometry[J].Journal of Pharmaceutical and Biomedical Analysis,2003,30(6):1773-1787.
[10]Toshimasa Toyo'oka,Masayoshi Kanbori,Yusuke Kumaki,et al.Detection of Triazolam and Its Hydroxy Metabolites in Rat Hair by Reversed-Phase Liquid Chromatography with Electrospray Ionization Mass Spectrometry[J].Journal of Analytical Toxicology,2000,24(3):194-201.
[11]孙雷,张骊,徐倩,等.超高效液相色谱-串联质谱法检测猪肉和猪肾中残留的10种镇静剂类药物[J].色谱,2010,28(1):38-42.
[12]许成保,锁然,张峰,等.超高效液相色谱-四极杆飞行时间质谱快速检测动物饲料中10种违禁精神药物[J].色谱,2012.30(5):457-462.
[13]索德成,赵根龙,李兰,等.液相色谱-串联质谱法同时检测饲料中7种精神类药物[J].分析化学研究简报,2010,38(7):1023-1026.
[14]严丽娟,张峰,吴敏,等.UPLC-ESI MS/MS法测定动物饲料中苯二氮卓类药物[J].分析测试学报,2011,30(11):1301-1305.
[15]Dennis J.Crouch,Douglas E.Rollins,Dennis V.Canfield,et al.Quantitation of Alprazolam and cz-Hydroxyalprazolam in Human Plasma Using Liquid Chromatography Electrospray Ionization MS-MS[J]Journal of Analytical Toxicology,1999,23(6):479-485.
[16]陈琴华,罗尚文,陈子林,等.HPLC-MS法同时测定5种抗癫痫药的血药浓度[J].中国科学:化学,2010,40(6):762-767.
[17]顾景凯,夏荣,钟大放,等。LC/MS~n法同时检测人尿液中艾司唑仑、阿普唑仑和三唑仑[J].药学学报,2002,37(2):138-140.