水产品中盐酸小檗碱的高效液相色谱-串联质谱法测定Determination of Berberine Hydrochloride Residues in Aquatic Products by High Performance Liquid Chromatography-mass Spectrometry(HPLC-MS/MS)
汤菊芬,王蓓,蔡佳,廖建萌,秦青英,黄月雄,简纪常
摘要(Abstract):
建立检测水产品中盐酸小檗碱残留量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经酸化甲醇(含体积分数1%甲酸)提取,正己烷脱脂,离心后,用高效液相色谱-串联质谱仪分析。以选择反应监测(SRM)正离子模式分析,定性离子对为336/320和336/292,定量离子对为336/320,盐酸小檗碱质量浓度在1~100 ng/mL范围内线性关系良好,线性相关系数为0.999 7,检出限为0.001 mg/kg。样品盐酸小檗碱的添加剂量为5~100μg/kg时,平均加标回收率为81.29%~104.06%,相对标准偏差为2.97%~7.87%,可满足水产品中盐酸小檗碱残留检测和药代动力学的研究需要。
关键词(KeyWords): 盐酸小檗碱;残留;水产品;高效液相色谱-串联质谱(HPLC-MS/MS)
基金项目(Foundation): 广东省科技计划(农业攻关)项目(2012B020308010);; 农业部公益性行业专项(20120385)
作者(Author): 汤菊芬,王蓓,蔡佳,廖建萌,秦青英,黄月雄,简纪常
参考文献(References):
- [1]杨先乐,陆承平,战文斌,等.新编渔药手册[M].北京:中国农业出版社,2005:217-218.
- [2]熊程亿,施绪保,代宗顺,等.3H-小檗碱在家兔及小鼠体内的药代动力学研究[J].中国药理学能报,1989,5(5):293-296.
- [3]余琛,张慧,潘俊芳,等.健康人口服黄连素片剂后的尿药分析与药物代谢初步研究[J].中国临床药理学杂志,2000,16(1):26-39.
- [4]温悦,贺英菊,罗巍伟.反高效液相色谱法测定兔血浆中盐酸小檗碱的浓度[J].中国药房,2005,16(12):900-901.
- [5]张丰青,杨中林,李萍.不同浓度和纯度盐酸檗碱大鼠肠道吸收动力比较研究[J].山东中医药大学学报,2008,32(6):506-509.
- [6]Miyazaki H,Shirai E,Ishibashi M,et al.Quantitative analysis of berberine in urine samples by chemical ionization mass fragmentography[J].Journal of Chromatography,1978,152(1):79-86.
- [7]Zuo F,Nakamura N,Akao T,et al.Pharmacokinetics of berberine and its main metabolites in conventional and pseudo germ-free rats determined by liquid chromatography/ion trap mass spectrometry[J].Drug Metabolism and Disposition,2006,34(12):2064-2072.
- [8]华雯妍,张全英,丁黎,等.LC-MS法研究健康人体盐酸小檗碱片的药代动力学[J].药学与临床研究,2009,17(6):465-468.
- [9]高海鹏,肖飞,马红伟,等.盐酸小檗碱在鸡体内的药动学研究[J].中国兽药杂志,2009,43(3):31-34.
- [10]王亮,叶小利,李学刚,等.黄连生物碱在大鼠体内的代谢转化及分布[J].中国中药杂志,2010,35(15):2017-2010.
- [11]肖学凤,乔晓莉,高岚,等.黄柏中盐酸小檗碱的药代动力学研究[J].天津中医药大学学报,2008,27(4):263-265.
- [12]Gupta P K,Hubbard M,Gurley B,et al.Validation of a liquid chromatography-tandem mass spectrometric assay for the quantitative determination of hydrastine and berberine in human serum[J].Pharm Biomed Anal,2009,49(4):1021-1026.
- [13]Liu Q F,Li Z D,Shi X J,et al.Determination of berberine,palmatine and jatrorrhizine in rabbit plasma by liquid chromatography-electrospray ionization-mass spectrometry[J].Pharm Biomed Anal,2011,56(5):1006-1015.
- [14]Liu Q F,Shi X J,Li Z D,et al.Pharmacokinetic comparisons of berberine and palmatine in normal and metabolic syndrome rats[J].Journal of Ethnopharmacology,2014,151(1):287-291.
- [15]Lu,T,Liang,Y,Song,J,et al.Simultaneous determination of berberine and palmatine in rat plasma by HPLC–ESI-MS after oral administration of traditional Chinese medicinal preparation Huang-Lian-Jie-Du decoction and the pharmacokinetic application of the method[J].Journal of pharmaceutical and biomedical analysis,2006,40(5):1218-1224.