Zhang Dan, Park Jin-A, Abd El-Aty A M, Kim Seong-Kwan, Cho Sang-Hyun, Zheng Weijia, Choi Jeong-Min, Shim Jae-Han, Chang Byung-Joon, Kim Jin-Suk, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.
Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, Giza, Egypt.
Biomed Chromatogr. 2017 Nov;31(11). doi: 10.1002/bmc.3996. Epub 2017 May 24.
An analytical method was developed for the detection of toldimfos sodium residues in porcine muscle and bovine milk using liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) analysis. The drug was extracted from muscle and milk using 10 mm ammonium formate in acetonitrile and then purified using n-hexane. The drug was well separated on a Luna C column using a mixture of 10 mm ammonium formate in ultrapure water (A) and acetonitrile (B) as the mobile phase. Good linearity was achieved over the tested concentration range (0.005-0.03 mg/kg) in matrix-matched standard calibration. The determination coefficients (R ) were 0.9942 and 0.9898 for muscle and milk, respectively. Fortified porcine muscle and bovine milk contained concentrations equivalent to and twice the limit of quantification (0.005 mg/kg) yielded recoveries in the range of 75.58-89.74% and relative standard deviations of ≤8.87%. Samples collected from large markets located in Seoul, Republic of Korea, tested negative for toldimfos sodium residue. In conclusion, ammonium formate in acetonitrile can effectively extract toldimfos sodium from porcine muscle and bovine milk without solid-phase extraction, which is usually required for cleanup before analysis. This method can be applied for the routine analysis of toldimfos in foods of animal origins.
建立了一种使用液相色谱 - 三重四极杆串联质谱(LC - MS/MS)分析法检测猪肌肉和牛乳中虫螨磷钠残留量的分析方法。使用乙腈中的10 mM甲酸铵从肌肉和牛奶中提取该药物,然后用正己烷进行纯化。在Luna C柱上,以超纯水(A)中的10 mM甲酸铵和乙腈(B)的混合物作为流动相,该药物得到了良好的分离。在基质匹配标准校准的测试浓度范围(0.005 - 0.03 mg/kg)内实现了良好的线性。肌肉和牛奶的测定系数(R)分别为0.9942和0.9898。在强化猪肌肉和牛乳中,浓度相当于定量限(0.005 mg/kg)和两倍定量限的回收率在75.58 - 89.74%范围内,相对标准偏差≤8.87%。从韩国首尔的大型市场采集的样本检测出虫螨磷钠残留呈阴性。总之,乙腈中的甲酸铵可以有效地从猪肌肉和牛乳中提取虫螨磷钠,无需进行通常在分析前用于净化的固相萃取。该方法可用于动物源性食品中虫螨磷的常规分析。