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

引用本文: 吕佳乐, 刘正才, 姚闽娜, 林元地. 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[J]. 色谱, 2020, 38(2): 212-217. doi: 10.3724/SP.J.1123.2019.04047 shu

Citation: LÜ Jiale, LIU Zhengcai, YAO Minna, LIN Yuandi. Determination of four protease inhibitors in chicken by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2020, 38(2): 212-217. doi: 10.3724/SP.J.1123.2019.04047 shu

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

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
基金项目:
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，3 μm），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0.1~20.0 μg/L范围内，4种目标化合物呈良好的线性关系，相关系数（r²）大于0.99，方法的定量限（S/N=10）为0.20~0.90 μg/kg；鸡肉组织中4种目标化合物在1.0、2.0和10.0 μg/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。

关键词:

English

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

1.
Food Science College of Fujian Agriculture and Forestry University, Fuzhou 350002, China;
2.
Technology center of Fuzhou Customs District, Fuzhou 350001, China
Received Date: 29 April 2019
Fund Project:
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China (No. 2014IK110)

Abstract: 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 (r²) 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.

Key words:

ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
/ solid phase extraction (SPE)
/ saquinavir
/ ritonavir
/ nelfinavir
/ indinavir
/ chicken

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

English

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

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