超高效液相色谱-串联质谱法测定鸡肉中4种蛋白酶抑制剂  

Determination of four protease inhibitors in chicken by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：吕佳乐 刘正才 姚闽娜[1] 林元地 Lü Jiale;LIU Zhengcai;YAO Minna;LIN Yuandi(Food Science College of Fujian Agriculture and Forestry University,Fuzhou 350002,China;Technology center of Fuzhou Customs District,Fuzhou 350001,China)

机构地区：[1]福建农林大学食品科学学院,福建福州350002 [2]福州海关技术中心,福建福州350001

出　　处：《色谱》2020年第2期212-217,共6页Chinese Journal of Chromatography

基　　金：国家质检总局科技项目(2014IK110);福建农林大学科技创新专项基金项目(CXZX2017013)~~

摘　　要：建立了鸡肉中4种蛋白酶抑制剂(沙奎那韦、利托那韦、奈非那韦、茚地那韦)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品经30%(v/v)乙腈水溶液(含1%(v/v)三氯乙酸)振荡提取、混合型阳离子交换MCX柱净化,采用Luna~? C8色谱柱(150 mm×2 mm, 3μm),以0.2%(v/v)甲酸水溶液(含5 mmol/L乙酸铵)和乙腈为流动相进行梯度洗脱,采用电喷雾电离(ESI^+)源和多反应监测(MRM)模式检测。结果表明,在0.1~20.0μg/L范围内,4种目标化合物呈良好的线性关系,相关系数(r^2)大于0.99,方法的定量限(S/N=10)为0.20~0.90μg/kg;鸡肉组织中4种目标化合物在1.0、2.0和10.0μg/kg 3个水平下的平均加标回收率为69.0%~106.0%,日内和日间相对标准偏差(RSD)为2.2%~13.8%(n=6)和3.6%~14.6%(n=3)。该法简单、高效、灵敏、准确,可用于鸡肉中沙奎那韦、利托那韦、奈非那韦、茚地那韦残留量的测定。A method was developed for the determination of four protease inhibitors(saquinavir, ritonavir, nelfinavir and indinavir) in chicken using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The samples were extracted by shaking with 30%(v/v) acetonitrile aqueous solution(containing 1%(v/v) trichloroacetic acid), and purified by using mixed-mode cationic-exchanger(MCX) cartridges. The samples were separated on a Luna~? C8 column(150 mm×2 mm, 3 μm) using 0.2%(v/v) formic acid aqueous solution(containing 5 mmol/L ammonium acetate) and acetonitrile as the mobile phases with gradient elution. The determination was carried out by using an electrospray ion source in the positive and multiple-reaction monitoring(MRM) modes. The calibration curves showed good linearities in the range of 0.1-20.0 μg/L, and the correlation coefficients(r^2) were greater than 0.99. The limits of quantification(LOQs, S/N=10) of the four protease inhibitors varied from 0.20 μg/kg to 0.90 μg/kg. At the spiked levels of 1.0, 2.0, and 10.0 μg/kg, the average recoveries of the four protease inhibitors were ranging from 69.0% to 106.0%. The intra-day and inter-day relative standard deviations(RSDs) were 2.2%-13.8%(n=6) and 3.6%-14.6%(n=3), respectively. The method is simple, efficient, sensitive and accurate, and it can be used to detect residues of saquinavir, ritonavir, nelfinavir and indinavir in chicken.

关 键 词：超高效液相色谱-串联质谱 固相萃取 沙奎那韦 利托那韦 奈非那韦 茚地那韦 鸡肉 

分 类 号：O658[理学—分析化学]