建立了测定畜禽肉中残留卡马西平的多波长可见吸收光谱法。在pH值3.59 Tris-HCl介质中,固绿FCF与卡马西平反应生成具有3个明显负吸收峰的绿色离子缔合物,出现褪色现象。最大负吸收峰位于660 nm,另2个负吸收峰分别位于558 nm和424 nm,线性范围均为0.05～3.8 mg/L,遵从比尔定律,它们的表观摩尔吸光系数(κ)分别为 6.74×104(660 nm)、5.71×104(558 nm)和5.13×104(424 nm)L/(mol·cm),定量限为0.11 mg/kg(660 nm)和 0.10 mg/kg(424 nm和558 nm)。当用双波长叠加(660 nm+558 nm)法测定时,其灵敏度为1.25×105 L/(mol·cm),定量限为0.053 mg/kg。当用三波长叠加(660 nm+558 nm+424 nm)法测定时,其灵敏度达1.76×105 L/(mol·cm),定量限为0.036 mg/kg。用灵敏度最高的三波长法测定生鲜畜禽肉中残留卡马西平含量,回收率为98.4%～102%,相对标准偏差(n=5)为2.4%～3.2%。
A new multi-wavelength visible absorption spectroscopy method for determining residual carbamazepine in livestock and poultry meat was established. In Tris-hydrochloric acid medium of pH=3.59, fast green FCF reacted with carbamazepine formed a green ion association complex with obvious three negative absorption peaks, and a faded phenomenon appeared in visible area. The maximum negative absorption peak was located at 660 nm, and the other two negative absorption peaks located at 558 nm and 424 nm, respectively. Their linear range were within 0.05-3.8 mg/L. Within this range, Beer's law was obeyed. Their apparent molar absorptivity (κ) were 6.74×104 (660 nm), 5.71×104 (558 nm), and 5.13×104 (424 nm) L/(mol·cm), respectively, with the quantitation limits being 0.11 mg/kg (660 nm) and 0.10 mg/kg (424 nm and 558 nm), respectively. When the double wavelength (660 nm+558 nm) superposition negative absorption spectrometry was used to determine the concentration of carbamazepine, its sensitivity attained 1.25×105 L/(mol·cm) and its quantitative limit was 0.053 mg/kg. When three-wavelength (660 nm+558 nm+424 nm) superposition negative absorption spectrometry was used to determine the concentration of carbamazepine, its sensitivity attained 1.76×105 L/(mol·cm) and its quantitative limit was 0.036 mg/kg. When the most sensitive three-wavelength method was applied to determine the content of residual carbamazepine in the livestock and poultry meat with spiked recoveries, the recovery and RSD% (n=5) were found to be in the ranges of 98.4%-102% and 2.4%-3.2%, respectively.
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