Kikuchi Hiroyuki, Sakai Takatoshi, Okura Tomoko, Nemoto Satoru, Akiyama Hiroshi, Taguchi Takaaki, Tsutsumi Tomoaki
National Institute of Health Sciences.
Graduate school of Pharmacy, Hoshi University.
Shokuhin Eiseigaku Zasshi. 2023;64(2):61-68. doi: 10.3358/shokueishi.64.61.
A simple and sensitive method for the determination of moenomycin A residues in livestock products using LC-MS/MS was developed. Moenomycin A, a residual definition of flavophospholipol, was extracted from samples with a mixture of ammonium hydroxide and methanol (1 : 9, v/v) preheated at 50℃. The crude extracted solutions were evaporated and purified by liquid-liquid partitioning between a mixture of ammonium hydroxide, methanol and water (1 : 60 : 40, v/v/v) and ethyl acetate. The alkaline layer was taken, and cleaned up using a strong anion exchange (InertSep SAX) solid phase extraction cartridge. The LC separation was performed on an Inertsil C8 column with liner gradient elution using 0.3 vol% formic acid and acetonitrile containing 0.3 vol% formic acid. Moenomycin A was detected using tandem mass spectrometry with negative ion electrospray ionization. Recovery tests were conducted using three porcine samples (muscle, fat and liver) and chicken eggs. Samples were spiked with moenomycin A at 0.01 mg/kg and at the Japanese Maximum Residue Limits (MRLs) established for each sample. The trueness ranged from 79 to 93% and precision ranged from 0.5 to 2.8%. The limit of quantification (S/N≥10) of the developed method is 0.01 mg/kg. The developed method would thus be very useful for regulatory monitoring of flavophospholipol in livestock products.
建立了一种使用液相色谱-串联质谱法测定畜产品中莫能菌素A残留量的简单灵敏方法。莫能菌素A是黄磷脂醇的残留定义物,用预热至50℃的氢氧化铵和甲醇(1:9,v/v)混合液从样品中提取。将粗提取液蒸发,并通过在氢氧化铵、甲醇和水(1:60:40,v/v/v)与乙酸乙酯的混合液之间进行液-液分配来纯化。取碱性层,并用强阴离子交换(InertSep SAX)固相萃取柱进行净化。液相色谱分离在Inertsil C8柱上进行,采用线性梯度洗脱,使用0.3%(体积)的甲酸和含0.3%(体积)甲酸的乙腈。使用负离子电喷雾电离串联质谱法检测莫能菌素A。使用三个猪样品(肌肉、脂肪和肝脏)和鸡蛋进行回收率测试。样品分别添加0.01 mg/kg的莫能菌素A以及针对每个样品设定的日本最大残留限量(MRLs)。准确度范围为79%至93%,精密度范围为0.5%至2.8%。所建立方法的定量限(S/N≥10)为0.01 mg/kg。因此,所建立的方法对于畜产品中黄磷脂醇监管监测非常有用。