超高效液相色谱-质谱内标法同时测定海洋药用生物中硝基呋喃类代谢物残留量

目的:建立测定海洋药用生物中4种硝基呋喃类药物(呋喃唑酮、呋喃它酮、呋喃西林和呋喃妥因)代谢物的超高效液相色谱-串联质谱方法。方法: 硝基呋喃类代谢物经过二硝基苯甲醛衍生化,用乙酸乙酯提取,经液相色谱分离,串联四极杆质谱多反应监测(MRM)模式检测,内标法定量。结果: 4种硝基呋喃类代谢物线性范围为0.5~20.0 μg·L^-1,相关系数均大于0.99,定量限在0.06~0.37 μg·kg^-1范围内,加标回收率为90.2%~101.6%,RSD为2.9%~4.8%。结论: 该方法前处理简单,灵敏度和准确度高,适合对海洋药用生物中硝基呋喃类代谢物残留的检测。

Objective: To develop a UPLC-MS/MS method for the simultaneous determination of four nitrofuran metabolites(furazolidone,furaltadone,nitrofurazone and nitrofurantoin)in marine drug organisms. Methods: Samples were derivatized with 2-nitrobenzaldehyde and extracted by ethyl acetate.The analytes were separated using UPLC and detected by multi-reactions monitoring(MRM)technology of tandem mass spectrometry with electrospray ionization source. Results: The calibration curve of four nitrofuran metabolites showed good linearity in the range of 0.5-20.0 μg·L^-1,and correlation coefficient were all above 0.99.The limits of quantification for four nitrofuran metabolites in samples were between 0.06 and 0.37 μg·kg^-1.The average recoveries at three levels(0.5、1.0、5.0 μg·kg^-1)ranged from 90.2 %-101.6 % with RSD 2.9 % to 4.8 %. Conclusion: The established method is simple,sensitive and accurate,which is suitable for the determination of four nitrofuran metabolites in marine drug organisms.

1 RONG Wei-guang(荣维广),GUO Hua(郭华),YANG Hong(杨红).Current research status in China on pesticide contamination of plant material used in making Chinese herbal medicines(我国中药材农药残留污染研究现状).Chin J Pestic(农药),2006,45(5):302
2 CHEN An-zhen(陈安珍),TIAN Jin-gai(田金改),DU Qing-peng(杜庆鹏).Study on method for rapid determination of organophosphorus and carbamates pesticide residues in traditional Chinese medicines(中药材中有机磷和氨基甲酸酯农药残留的快速检测方法).Chin Pharm Aff(中国药事),2009,23(11):1063
3 DU Qing-peng(杜庆鹏),CHEN An-zhen(陈安珍),TIAN Jin-gai(田金改),et al.Study on method for rapid determination of cadmium(Ⅱ)in traditional Chinese medicines(中药材中重金属镉的快速检测方法研究).Chin Pharm Aff(中国药事),2011,25(8):776
4 DU Qing-peng(杜庆鹏),CHEN An-zhen(陈安珍),TIAN Jin-gai(田金改),et al.Study on method for rapid determination of mercury in traditional Chinese medicines(中药材中重金属汞快速检测试纸方法研究). Chin Pharm Aff(中国药事),2010,24(12):1175
5 SHE Yong-xin(佘永新),LI Bao-hai(李宝海),CAO Wei-qiang(曹维强), et al.Progress on the determination methods for nitrofuran antibiotics and their metabolites residues in animal foods(动物性食品中硝基呋喃类药物及其代谢物残留检测技术的研究进展).Mod Sci Instrum(现代科学仪器),2010,12(6):149
6 LIU Si-xin(刘四新),HU Xian-e(胡先娥),LIN Zheng-feng(林正峰),et al.Improved liquid chromatography-tandem mass spectrometric method for determination of nitrofuran metabolites residues in aquatic products(液相色谱串联质谱法检测水产品硝基呋喃类代谢物的改进).J Food Sci(食品科学),2009,30(20):331
7 WANG Jing(王璟),YANG Nan(杨楠),ZHAO Jing(赵晶)),et al.Determination of metabolites of nitrofuran antibiotics in aquatic products by high-performance liquid chromatography-tandem mass spectrometry(液相色谱 -串联质谱法检测水产品中硝基呋喃类代谢物).Chin J Health Lab Technol(中国卫生检验杂志),2008,18(6):978
8 Method for the determination residues of the metabolites of nitrofuran in pork beef chicken porcine liver and aquatic products-LC-MS-MS method(猪肉、牛肉、鸡肉、猪肝和水产品中硝基呋喃类代谢物残留量的测定液相色谱-串联质谱法).GB/T 20752-2006
9 CHEN Tao(陈涛),CHEN An-zhen(陈安珍),YANG Zhao(杨钊).UPLC-MS/MS determination of 11 quinolone residuces in animal products(超高效液相色谱- 串联质谱法测定动物源产品中11种喹诺酮类药物残留).Chin J Pharm Anal (药物分析杂志),2010,30( 6):1087