高效液相色谱法同时测定中毒患者血清中5种精神活性物质的浓度

doi:10.3969/j.issn.1006-7795.2013.02.020

首都医科大学学报 ›› 2013, Vol. 34 ›› Issue (2): 270-274.doi: 10.3969/j.issn.1006-7795.2013.02.020

高效液相色谱法同时测定中毒患者血清中5种精神活性物质的浓度

果伟¹, 赵晔¹, 郭桂欣¹, 张军¹, 孙川¹, 荣璋¹, 段晓霞², 李文标¹, 翟屹民¹

1. 首都医科大学附属北京安定医院临床精神药理实验室, 北京 100088;
2. 太原精神病医院检验科, 山西太原 030045

收稿日期:2012-08-24 出版日期:2013-04-21 发布日期:2013-04-17
通讯作者: 翟屹民 E-mail:zhai_yimin@yahoo.com.cn
基金资助:
北京市委组织部优秀人才培养专项基金(2004);首都医学科研发展基金(2009-3135)。

Simultaneous determination of five psychoactive drugs in overdosed patients serum by high performance liquid chromatography

GUO Wei¹, ZHAO Ye¹, GUO Guixin¹, ZHANG Jun¹, SUN Chuan¹, RONG Zhang¹, DUAN Xiaoxia², LI Wenbiao¹, ZHAI Yimin¹

1. Laboratory of Clinical Psychopharmacological, Beijing Anding Hospital, Capital Medical University, Beijing 100088, China;
2. Department of Clinical Chemistry, Psychiatric Hospital of Taiyuan, Taiyuan 030045, Shanxi Province China

Received:2012-08-24 Online:2013-04-21 Published:2013-04-17
Supported by:
This study was supported by Talents Fund of Beijing Municipal Party Committee Organization Department(2004); Capital Medical Research and Development Fund(2009-3135).

摘要/Abstract

摘要：

目的建立可同时测定人血清中利培酮、9-羟利培酮、氯氮平、去甲氯氮平和瑞波西汀5种药物浓度的高效液相色谱-紫外检测法,并将该方法用于临床急性精神药物中毒患者的血液样本分析。方法以乙醚为溶剂进行一步液液萃取,待测物与内标帕罗西汀在Inertsil ODS-3柱,乙腈: 甲醇: 正丁胺: 冰醋酸: 去离子水(20: 2.87: 1.07: 1: 34.29)条件下可以基线分离。线性范围100~1 600 ng/mL,最低检测限25 μg/L(S/N=10)。结果本方法批内精密度为3.1%~15.6%,批间精密度为5.7%~18.4%;批内准确度为0.1%~8.7%,批间准确度为0.3%~13.3%。常见精神科药物不干扰待测药物和内标。结论本方法简单、特异性好,可应用于急诊患者药物中毒检测。

关键词: 过量中毒, 液液萃取, 高效液相色谱

Abstract:

Objective A high performance liquid chromatography(HPLC) method with ultraviolet(UV) detection(230 nm) was developed and validated for the quantification of 5 drugs, Risperidone, clozapine, reboxetine, 9-hydroxy Risperidone and norclozapine, in human serum. Methods Following a one-step liquid-liquid extraction with diethyl ether, the analyte and internal standard(paroxetine) were separated using an isocratic mobile phase consisted of acetonitrile: methanol: butylamine: acetic acid: deionized water=20: 2.9: 1.1: 1: 34.3 on a reverse phase Inertsil C₁₈-3 column. Five drugs and IS were separated well under the chromatographic condition. The calibration curve was verified over the range of 100~1 600 μg/L and limit of detection(LOD) was 25 μg/L(S/N=10). Results The imprecision of within and between batches were 3.1%~15.6% and 5.7%~18.4%, respectively. The accuracy of within and between batches were 0.1%~8.7% and 0.3%~13.3%. Commonly used psychotropic drugs did not interfere with the drugs and internal standard. Conclusion This method was found to be rapid, simple, accurate, sensitive and more suitable for rapid qualitative and quantitative determination of drugs in the serum of overdosed patients.

Key words: overdose, liquid-liquid extraction, high performance liquid chromatography

中图分类号:

R971⁺.41

果伟, 赵晔, 郭桂欣, 张军, 孙川, 荣璋, 段晓霞, 李文标, 翟屹民. 高效液相色谱法同时测定中毒患者血清中5种精神活性物质的浓度[J]. 首都医科大学学报, 2013, 34(2): 270-274.

GUO Wei, ZHAO Ye, GUO Guixin, ZHANG Jun, SUN Chuan, RONG Zhang, DUAN Xiaoxia, LI Wenbiao, ZHAI Yimin. Simultaneous determination of five psychoactive drugs in overdosed patients serum by high performance liquid chromatography[J]. Journal of Capital Medical University, 2013, 34(2): 270-274.

参考文献

[1] Kwatra S G, Batson N E, Kramer S I. Long-acting risperidone and oral antipsychotics in schizophrenia[J]. N Engl J Med, 2011,364(23):2264-2265, 265-266.

[2] Eyding D, Lelgemann M, Grouven U, et al. Reboxetine for acute treatment of major depression: systematic review and meta-analysis of published and unpublished placebo and selective serotonin reuptake inhibitor controlled trials[J]. BMJ, 2010,341:c4737.

[3] 苏金哥,郭红丽,王秀芳,等.精神药物的不良反应[J].临床精神医学杂志,2012,1:69-70.

[4] 孙成文,王汉斌,等.精神药物中毒的快速定性检测[J].中华精神科杂志,2001,34(4):239.

[5] 张梦琪,贾晶莹,陆晓佩,等.LC-MS/MS同时测定人血清中5种抗精神类药物和9种抗抑郁药物的浓度[J].中国药学杂志,2011,46(1):51-60.

[6] Rao L V, Snyder M L, Vallaro G M. Rapid liquid chromatography/tandem mass spectrometer(LCMS) method for clozapine and its metabolite N-desmethyl clozapine(norclozapine) in human serum[J]. J Clin Lab Anal, 2009,23(6):394-398.

[7] Locatelli I, Mrhar A, Grabnar I. Simultaneous determination of risperidone and 9-hydroxyrisperidone enantiomers in human blood plasma by liquid chromatography with electrochemical detection[J]. J Pharm Biomed Anal, 2009,50(5):905-910.

[8] 尹明兰.HPLC法同时监测5种抗精神病药血药浓度[J].中国药房,2007,18(11):837-838.

[9] Ragg M A, Mandrioli R, Casamenti G, et al. Determination of reboxetine, a recent antidepressant drug, in human plasma by means of two high-performance liquid chromatography methods[J]. J Chromatogr A, 2002,949(1-2):23-33.

[10] 国家药典委员会.中华人民共和国药典(二部)[M].北京:中国医药科技出版社,2010.

[11] 张剑萍,郭澄.生物样品分析中的方法学验证[J].中国药房,2008(31):2469-2471.

[12] Hiemke C, Baumann P, Bergemann N, et al. AGNP consensus guidelines for therapeutic drug monitoring in psychiatry: update 2011[J]. Pharmacopsychiatry, 2011,44(6):195-235.

[13] 周小东,付华斌,刘知源,等.新型抗精神病药物研发过程中面临的问题和解决方案[J].解放军医药杂志,2012,24(2):33-37.

[14] 郑晓人,高镇松,刘南华,等.抗精神病药物中毒患者的精神心理和个性研究[J].中国煤炭工业医学杂志,2010,13(5):669-671.

[1]	李鹏飞, 范家明, 刘河, 张茜, 安卓玲, 刘丽宏. 大鼠体内百草枯组织分布研究[J]. 首都医科大学学报, 2019, 40(5): 726-730.
[2]	杨一帆, 秦一, 徐唯哲, 徐平湘, 薛明. 吡硫醇在低氧与常氧环境下大鼠体内的药代动力学研究[J]. 首都医科大学学报, 2017, 38(2): 232-237.
[3]	秦春雨, 周滔, 宫雯雯, 白露, 秦一, 徐唯哲, 徐平湘, 王晓民, 薛明. UPLC-MS/MS法测定大鼠血浆中雷公藤内酯醇及其药代动力学[J]. 首都医科大学学报, 2015, 36(1): 121-126.
[4]	刘相佟, 王友信, 杨兴华, 董晶, 王嵬, 郭秀花. 不同年龄段人群蛋白质N-糖基的结构谱型研究[J]. 首都医科大学学报, 2014, 35(6): 779-784.
[5]	李鹏飞, 王淑民, 张茜, 安卓玲, 刘丽宏. LC-MS/MS法测定人血浆中氨基葡萄糖的浓度[J]. 首都医科大学学报, 2013, 34(5): 715-719.
[6]	杨荟敏;祝佳玮;赵宸龙;张晨光;张红;赵文明. HPLC法同时检测血浆中半胱氨酸/胱氨酸和还原型谷胱甘肽/氧化型谷胱甘肽的氧化还原电势[J]. 首都医科大学学报, 2012, 33(1): 84-88.
[7]	肖引;刘凯;陈江;彭国华;李广琪;陈芳;李勃;闫美娟. 参七复脉片质量控制标准的研究及确定[J]. 首都医科大学学报, 2011, 32(5): 650-652.
[8]	夏彬彬;李伊莎;徐唯哲;王桥;宋学英. 积雪草中积雪草酸的分离、纯化及其含量测定[J]. 首都医科大学学报, 2011, 32(4): 538-540.
[9]	吴燕川;李尧华;谢胜男;李昕;于顺;何士大. 液相色谱法测定小鼠脑组织中ATP、ADP及AMP含量[J]. 首都医科大学学报, 2011, 32(4): 534-537.
[10]	郜文;丁兆毅;徐菲;郭建强. HPLC法测定大枣环磷酸腺苷（c-AMP）的含量[J]. 首都医科大学学报, 2011, 32(3): 375-378.
[11]	赵淑锐;徐艳霞;徐菲;郜文. 检测中草药提取物中黄曲霉毒素的高灵敏方法[J]. 首都医科大学学报, 2011, 32(3): 379-383.
[12]	赵逸松;崔歆;梁堃;刘爽;杨琳;赵峰. 高效液相色谱-质谱联用分析法测定血清全氟辛烷磺酸[J]. 首都医科大学学报, 2009, 30(3): 336-340.
[13]	殷志爽;赵文华;宋学英;孔令江;王桥. HPLC法测定白芍和赤芍中1,2,3,4,6-五-O-倍酰-D-葡萄糖含量[J]. 首都医科大学学报, 2008, 29(5): 601-604.
[14]	张军;李文标;郭桂欣;翟屹民;果伟;王传跃. HPLC紫外检测法测定血浆甲磺酸瑞波西汀浓度[J]. 首都医科大学学报, 2008, 29(4): 431-435.
[15]	李长勇;姜向明;俞豪;李丽英. 高效液相色谱法测定生物样品中磷酸鞘氨醇的含量[J]. 首都医科大学学报, 2008, 29(4): 459-462.

高效液相色谱法同时测定中毒患者血清中5种精神活性物质的浓度

Simultaneous determination of five psychoactive drugs in overdosed patients serum by high performance liquid chromatography

PDF

可视化

被引次数

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价