Cho Hee-Jung, Jo Kyul, Yi Hee, Cho Soo Min, Abd El-Aty A M, Kim Min Kyung, Han Sang Beom, Oh Jae Ho, Kwon Chan Hyeok, Shim Jae-Han, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, 1 Hwayang-dong, Kwangjin-gu, Seoul, 143-701, Republic of Korea.
Biomed Chromatogr. 2011 Sep;25(9):1061-6. doi: 10.1002/bmc.1579. Epub 2011 Mar 14.
In this work, a liquid chromatography-tandem mass spectrometric detection technique was developed and validated for the determination of brotizolam residues in beef muscle and commercial whole milk. This procedure involves the extraction of the analyte from the samples via liquid-solid extraction, and caffeine was used as an internal standard. The analyte was successfully separated on an XTerra-C(18) column, with a mobile phase composed of 0.01% formic acid in acetonitrile and 1 mm ammonium formate-0.01% formic acid in water. The one-step extraction method evidenced good selectivity, precision (RSD = 9.87-26.47%), and the recovery of the extractable analyte was 92.61-115.98% in the matrices. The limits of quantification ranged between 0.4 and 0.5 µg/kg. The developed method is simple since it requires no additional cleanup procedures.
在本研究中，开发并验证了一种液相色谱 - 串联质谱检测技术，用于测定牛肉肌肉和市售全脂牛奶中的溴替唑仑残留量。该方法通过液 - 固萃取从样品中提取分析物，并使用咖啡因作为内标。分析物在XTerra - C(18)柱上成功分离，流动相由乙腈中0.01%的甲酸和水中1 mM甲酸铵 - 0.01%的甲酸组成。一步萃取法具有良好的选择性、精密度（相对标准偏差 = 9.87 - 26.47%），且在基质中可萃取分析物的回收率为92.61 - 115.98%。定量限在0.4至0.5 µg/kg之间。所开发的方法简单，因为它无需额外的净化步骤。
