Inoue Koichi, Yoshimi Yukiko, Hino Tomoaki, Oka Hisao
Department of Physical and Analytical Chemistry, School of Pharmacy, Kinjo Gakuin University, 2-1723 Omori, Moriyama-ku, Nagoya 463-8521, Japan.
Shokuhin Eiseigaku Zasshi. 2010;51(1):1-9. doi: 10.3358/shokueishi.51.1.
An LC/ESI (positive-mode)-MS/MS method was developed for simultaneous quantification of 8 macrocyclic lactones (abamectin B1a, abamectin 8,9-Z isomer B1a, emamectin benzoate B1a, emamectin benzoate 8,9-Z isomer B1a, ivermectin, eprinomectin B1a, doramectin and moxidectin) in animal tissues, egg, milk and honey. The separation was achieved on a TSK-GEL ODS 100 V column (2.0 x 50 mm, 3 microm) with a mobile phase consisting of 0.1% formic acid in acetonitrile, and 0.1 mM ammonium formate-0.1% formic acid in water, at a flow rate of 0.2 mL/min with gradient elution. Linear calibration plots were obtained with high correlation coefficients (r=0.998-0.999). The LOQ and LOD ranged from 0.02-1.5 ng/mL and 0.1-5 ng/mL, respectively. Average recoveries were in the range of 70.8-117.1% with associated RSD values<15% (n=10) for repeatability and reproducibility. The spiking levels for recoveries and RSDs met the validation criteria for Japanese maximum residue limits (MRLs). Based on these results, the proposed analytical method has been proven to be highly efficient and suitable for routine determinations of macrocyclic lactones in animal food matrices.
建立了一种液相色谱/电喷雾电离（正离子模式）-串联质谱法，用于同时定量分析动物组织、蛋类、奶类和蜂蜜中的8种大环内酯类药物（阿维菌素B1a、阿维菌素8,9-Z异构体B1a、甲氨基阿维菌素苯甲酸盐B1a、甲氨基阿维菌素苯甲酸盐8,9-Z异构体B1a、伊维菌素、埃普利诺菌素B1a、多拉菌素和莫西菌素）。采用TSK-GEL ODS 100 V柱（2.0×50 mm，3μm）进行分离，流动相由乙腈中0.1%甲酸和水中0.1 mM甲酸铵-0.1%甲酸组成，流速为0.2 mL/min，梯度洗脱。获得了具有高相关系数（r=0.998-0.999）的线性校准曲线。定量限和检测限分别为0.02-1.5 ng/mL和0.1-5 ng/mL。平均回收率在70.8-117.1%范围内，重复性和再现性的相关相对标准偏差值<15%（n=10）。回收率和相对标准偏差的加标水平符合日本最大残留限量（MRLs）的验证标准。基于这些结果，所提出的分析方法已被证明高效且适用于动物食品基质中大环内酯类药物的常规测定。
