鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备

doi:10.16431/j.cnki.1671-7236.2015.09.009

《中国畜牧兽医》---唯一指定的官方网站 ›› 2015, Vol. 42 ›› Issue (9): 2278-2285.doi: 10.16431/j.cnki.1671-7236.2015.09.009

鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备

常平平¹, 许春南¹, 张立新², 郝小妹¹, 高兴¹, 陈超¹

1. 北京勤邦生物技术有限公司, 北京 102206;
2. 北京市优质农产品产销服务站, 北京 100101

收稿日期:2015-01-26 出版日期:2015-09-20 发布日期:2015-09-25
通讯作者: 陈超 E-mail:chenchao@kwinbon.com
作者简介:常平平(1984-),女,山西晋城人,硕士,化学分析工程师,研究方向:食品安全检测技术,E-mail:cpp19840911@163.com
基金资助:
国家重大科学仪器设备开发专项"全自动化学发光免疫分析仪工程化开发及应用(2013YQ140371)

Establishment of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Determination Method of Amantadine in Chicken and Preparation of Positive Samples

CHANG Ping-ping¹, XU Chun-nan¹, ZHANG Li-xin², HAO Xiao-mei¹, GAO Xing¹, CHEN Chao¹

1. Beijing Kwinbon Biotechnology Co., Ltd., Beijing 102206, China;
2. Beijing Quality Agricultural Production and Marketing Service Station, Beijing 100101, China

Received:2015-01-26 Online:2015-09-20 Published:2015-09-25

摘要/Abstract

摘要： 本试验建立了一种超高效液相色谱—电喷雾串联质谱测定鸡肉中金刚烷胺的分析方法。以甲醇-1%三氯乙酸作提取剂,采用超声波辅助溶剂萃取法萃取鸡肉中金刚烷胺,萃取液用MCX固相萃取柱进行净化浓缩。以BEH C18色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。对质谱和色谱条件、提取剂的种类、超声提取时间、固相萃取柱及洗脱液的种类进行了优化,在0.1~20.0 ng/mL范围内线性关系良好(r=0.9998)。样品在5.0、10.0 和20.0 μg/kg添加水平的回收率为89.7%~101.4%,相对标准偏差(RSD)小于7.0%;方法的检测限为0.07 μg/kg,定量限为0.23 μg/kg。本方法灵敏度高、准确度高,能满足公司及相应鸡肉行业的客户进行鸡肉中金刚烷胺残留量的快速、高灵敏检测分析。本试验还根据金刚烷胺在动物体内的代谢动力学成功制备了浓度为11.16和7.18 mg/kg的金刚烷胺阳性鸡肉样品,为研发金刚烷胺ELISA试剂盒提供了相应的阳性样品。

关键词: 超高效液相色谱— 电喷雾串联质谱; 金刚烷胺; 鸡肉; 阳性样品

Abstract: An ultra performance liquid chromatography (UPLC)-tandem mass spectrometry analysis method was established in this experiment for determination of amantadine in chicken.1% trichloroacetic acid with methanol as extraction liquid, the ultrasonic assisted solvent extraction was used to extract amantadine in chicken, extract liquid was purified and enriched in MCX solid-phase extraction column.Using C18 chromatographic column as separation column, in the positive ion mode, we detected the samples by electrospray ionization tandem mass spectrometry.Mass spectrometry and chromatographic conditions, the type of extract liquid, ultrasonic extraction time, the types of solid-phase extraction column and eluent were optimized.Under optimal conditions, a good linearity (r=0.9998) in the ranges of 0.1 to 20.0 ng/mL was obtained, the recoveries were 89.7% to 101.4% in the additive levels of 5.0, 10.0 and 20.0 μg/kg, the limit of detection (LOD) of amantadine was 0.07 μg/kg, the limit of quantiation (LOQ) of amantadine was 0.23 μg/kg, and the relative standard deviations (RSD) were below 7.0%.This novel approach had high sensitivity and accuracy, and was successfully applied to rapid and high sensitive detection of amantadine residues in chicken.The positive samples of amantadine in chicken were successfully prepared with concentrations of 11.16 and 7.18 mg/kg, which could be used for the research of ELISA kits of amantadine.

Key words: ultra performance liquid chromatography-tandem mass spectrometry; amantadine; chicken; positive sample

中图分类号:

S852.4

常平平, 许春南, 张立新, 郝小妹, 高兴, 陈超. 鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备[J]. 《中国畜牧兽医》---唯一指定的官方网站, 2015, 42(9): 2278-2285.

CHANG Ping-ping, XU Chun-nan, ZHANG Li-xin, HAO Xiao-mei, GAO Xing, CHEN Chao. Establishment of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Determination Method of Amantadine in Chicken and Preparation of Positive Samples[J]. , 2015, 42(9): 2278-2285.

参考文献

[1] Morrison D,Roy S,Rayner C,et al.A randomized,crossover study to evaluate the pharmacokinetics of amantadine and oseltamivir administered alone and in combination[J].PLoS One,2007,2(12):e1305.

[2] Narasimhachari N,Helgeson E,Prakash U.GC-MS-SIM quantitation of amantadine in biological samples[J].Chromatographia,1979,12(8):523-526.

[3] Leis H J,Fauler G,Windischhofer W J.Quantitative analysis of memantine in human plasma by gas chromatography/negative ion chemical ionization[J].Mass Spectrometry,2002,37(5):477-480.

[4] Cui S J,Feng F,Liu H,et al.New method for high-performance liquid chromatographic determination of amantadine and its analogues in rat plasma[J]. J Pharm Biomed Anal,2007,44(5):1100-1105.

[5] Higashi Y,Fujii Y.Simultaneous determination of the binding of amantadine and its analogues to synthetic melanin by liquid chromatography after precolumn derivatization with dansyl chloride[J].J Chromatogr Sci,2005,43(4):213-217.

[6] Higashi Y,Nakamura S,Matsumura H.Simultaneous liquid chromatographic assay of amantadine and its four related compounds in phosphate-buffered saline using 4-fluoro-7-nitro-2,1,3-benzoxadiazole as a fluorescent derivatization reagent[J].Biomed Chromatogr,2006,20(5):423-428.

[7] 张文伟,杨梅,施杰,等.荧光法测定片剂中金刚烷胺的含量[J].分析化学,2002,30(4):508.

[8] Feng S,Tian Y,Zhang Z.Rapid simultaneous determination of paracetamol,amantadine hydrochloride,caffeine and chlorpheniramine maleate in human plasma by liquid chromatography/tandem mass spectrometry[J].Arzneimittelforschung,2009,59(2):86-95.

[9] Arndt T,Guessregen B,Hohl A,et al.Determination of serum amantadine by liquid chromatography-tandem mass spectrometry[J].Clin Chim Acta,2005,359(1-2):125-131.

[10] Wang P,Liang Y Z,Chen B M,et al.Quantitative determination of amantadine in human plasma by liquid chromatography-mass spectrometry and the application in a bioequivalence study[J].J Pharm Biomed Anal,2007,43(4):1519-1525.

[11] 李士敏,王玮.液相色谱-质谱联用法测定大鼠血浆中盐酸金刚烷胺浓度及体内药动学研究[J].药物分析杂志,2007,27(1):66-68.

[12] Xu M J,Ju W Z,Xia X Y.Determination of rimantadine in rat plasma by liquid chromatography/electrospray mass spectrometry and its application in a phar macokinetic study[J].J Chromatogr B,2008,864(1-2):123-128.

[13] 云环,张朝晖,罗生亮,等.固相萃取LC-MS/MS法检测动物源性食品中的金刚烷胺[J].现代仪器,2009,15(6):42-45.

[14] GB/T 17025-2006.检测和校准实验室能力的通用要求[S].

[15] GB/T 27404-2008.实验室质量控制规范食品理化检测[S].

鸡肉中金刚烷胺超高效液相色谱-电喷雾串联质谱检测方法的建立及阳性样品的制备

Establishment of Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Determination Method of Amantadine in Chicken and Preparation of Positive Samples

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