Department of Sanitary Inspection, School of Public Health, Hebei Medical University, Shijiazhuang 050017, China.
Technology Center of Shijiazhuang Customs, Shijiazhuang 050051, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2021 May 1;1171:122637. doi: 10.1016/j.jchromb.2021.122637. Epub 2021 Mar 9.
A high throughput method was developed and validated for the quantitation of gamithromycin residues in eggs, milk and animal tissues (leg muscle, kidney, liver and fat) of different species and genera. This was undertaken using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The samples were extracted with acetonitrile and purified using an Oasis MCX solid phase extraction cartridge. Subsequently, a C18 column was used for chromatographic separation using acetonitrile and 0.1% formic acid as the mobile phase. LC-MS/MS in positive ESI and multiple reaction monitoring mode with gamithromycin-D4 as the internal standard was used for detection and quantification of gamithromycin. The method was successfully calibrated in the range of 1.0-200 µg/kg. The limit of detection (LOD) and limit of quantification (LOQ) for gamithromycin was 0.30-0.40 µg/kg and 0.80 - 1.0 µg/kg, respectively. The average recoveries of the analyte fortified at three levels ranged from 84.2% to 115.9%, with a relative standard deviation <10%. The proposed method has been successfully used to monitor real samples, and shown to be sensitive, rapid, and convenient. Hence, this method could be used for regulatory purposes to screen for the presence of gamithromycin residues in eggs, milk and target tissues.
建立并验证了一种高通量方法,用于定量检测不同物种和属的鸡蛋、牛奶和动物组织(腿部肌肉、肾脏、肝脏和脂肪)中的加米霉素残留。该方法采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)。样品用乙腈提取,并用 Oasis MCX 固相萃取小柱进行净化。然后,使用 C18 柱,以乙腈和 0.1%甲酸为流动相进行色谱分离。采用正电喷雾和多反应监测模式的 LC-MS/MS 检测和定量加米霉素,并用加米霉素-D4 作为内标。该方法在 1.0-200 µg/kg 的范围内成功校准。加米霉素的检测限(LOD)和定量限(LOQ)分别为 0.30-0.40 µg/kg 和 0.80-1.0 µg/kg。在三个添加水平下,分析物的平均回收率在 84.2%至 115.9%之间,相对标准偏差<10%。该方法已成功用于监测实际样品,并表现出灵敏、快速和方便的特点。因此,该方法可用于监管目的,以筛选鸡蛋、牛奶和目标组织中加米霉素残留。