Wen Dehui, Shi Rong, He Haiming, Chen Rundong, Zhang Yingzi, Liu Rong, Chen Hong
National Reference Laboratory of Veterinary Drug Residues, Guangdong Provincial Key Laboratory of Veterinary Pharmaceutics Development and Safety Evaluation, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China.
Quality Supervision, Inspection and Testing Center for Domestic Animal Products (Guangzhou), Ministry of Agriculture and Rural Affairs, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China.
Foods. 2023 May 29;12(11):2180. doi: 10.3390/foods12112180.
This study aimed to determine promethazine (PMZ) and its metabolites, promethazine sulfoxide (PMZSO) and monodesmethyl-promethazine (NorPMZ), in swine muscle, liver, kidney, and fat. A sample preparation method and high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis were established and validated. The samples were extracted using 0.1% formic acid-acetonitrile and purified with acetonitrile-saturated n-hexane. After concentration by rotary evaporation, the extract was re-dissolved in a mixture of 0.1% formic acid-water and acetonitrile (80:20, /). Analysis was performed using a Waters Symmetry C column (100 mm × 2.1 mm i.d., 3.5 μm) with 0.1% formic acid-water and acetonitrile as the mobile phase. The target compounds were determined using positive ion scan and multiple reaction monitoring. PMZ and NorPMZ were quantified with deuterated promethazine (PMZ-d6) as the internal standard, while PMZSO was quantified using the external standard method. In spiked muscle, liver, and kidney samples, the limits of detection (LOD) and limits of quantification (LOQ) for PMZ and PMZSO were 0.05 μg/kg and 0.1 μg/kg, respectively, while for NorPMZ, these values were 0.1 μg/kg and 0.5 μg/kg, respectively. For spiked fat samples, the LOD and LOQ for all three analytes were found to be 0.05 μg/kg and 0.1 μg/kg, respectively. The sensitivity of this proposed method reaches or exceeds that presented in previous reports. The analytes PMZ and PMZSO exhibited good linearity within the range of 0.1 μg/kg to 50 μg/kg, while NorPMZ showed good linearity within the range of 0.5 μg/kg to 50 μg/kg, with correlation coefficients (r) greater than 0.99. The average recoveries of the target analytes in the samples varied from 77% to 111%, with the precision fluctuating between 1.8% and 11%. This study developed, for the first time, an HPLC-MS/MS method for the determination of PMZ, PMZSO, and NorPMZ in four swine edible tissues, comprehensively covering the target tissues of monitoring object. The method is applicable for monitoring veterinary drug residues in animal-derived foods, ensuring food safety.
本研究旨在测定猪肌肉、肝脏、肾脏和脂肪中的异丙嗪（PMZ）及其代谢物异丙嗪亚砜（PMZSO）和去甲基异丙嗪（NorPMZ）。建立并验证了一种样品制备方法和高效液相色谱 - 串联质谱（LC - MS/MS）分析方法。样品用0.1%甲酸 - 乙腈提取，并用乙腈饱和正己烷纯化。经旋转蒸发浓缩后，提取物重新溶解于0.1%甲酸 - 水和乙腈（80:20，v/v）的混合溶液中。使用沃特世Symmetry C柱（100 mm×2.1 mm内径，3.5μm）进行分析，以0.1%甲酸 - 水和乙腈作为流动相。采用正离子扫描和多反应监测测定目标化合物。PMZ和NorPMZ以氘代异丙嗪（PMZ - d6）作为内标进行定量，而PMZSO采用外标法进行定量。在加标肌肉、肝脏和肾脏样品中，PMZ和PMZSO的检测限（LOD）和定量限（LOQ）分别为0.05μg/kg和0.1μg/kg，而NorPMZ的这些值分别为0.1μg/kg和0.5μg/kg。对于加标脂肪样品，所有三种分析物的LOD和LOQ分别为0.05μg/kg和0.1μg/kg。本方法的灵敏度达到或超过先前报道的方法。分析物PMZ和PMZSO在0.1μg/kg至五十μg/kg范围内表现出良好的线性，而NorPMZ在0.5μg/kg至五十μg/kg范围内表现出良好的线性，相关系数（r）大于0.99。样品中目标分析物的平均回收率在77%至111%之间，精密度在1.8%至11%之间波动。本研究首次建立了一种用于测定猪四种可食用组织中PMZ、PMZSO和NorPMZ的HPLC - MS/MS方法，全面覆盖了监测对象的目标组织。该方法适用于监测动物源性食品中的兽药残留，确保食品安全。
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