Ishikawa Fusako, Shigeoka Sutemi, Nagashima Machiko, Takahashi Misako, Kamimura Hisashi
Tokyo Metropolitan Research Laboratory of Public Health, 3-24-1 Hyakunin-cho, Shinjuku-ku, Tokyo 169-0073, Japan.
J AOAC Int. 2003 Mar-Apr;86(2):215-21.
A 3-step extraction method was developed for the simultaneous determination of 11 dyes and their aluminum lakes in drugs. The dyes were first extracted with warm water (approximately 60 degrees C) and were cleaned up by solid-phase extraction with a tC18 cartridge. Aluminum lake dyes that remained in the precipitate were extracted with 0.02M NaOH. Aluminum in the dye lakes was reextracted into the organic layer with acetylacetone-butyl acetate (1 + 9, v/v), as an acetylacetone chelate, and was quantified by atomic absorption spectrometry. The dye portions of the aluminum lakes remained in the aqueous layer and were cleaned up in the same way as the dyes. The dyes and the dye portions of the aluminum lakes were quantified by ion-pair liquid chromatography with a photodiode array detector within 20 min. The recoveries of dyes from drug fortified at 10 microg of each dye per pill were 87.0-102.2%, and the recoveries of dyes from drugs fortified at 50 microg of each dye lake per pill were 82.9-101.6%, except for recoveries of indigo carmine. In 40 ethical and over-the-counter drugs, dyes that were not indicated in the package insert information for drugs were detected in 5 samples. The highest amount of dye found in a drug was 1169.5 microg erythrosine, which was detected in a capsule of antibiotic. Aluminum lake dyes were detected in 8 samples of various dosage forms.
开发了一种三步萃取方法，用于同时测定药物中的11种染料及其铝色淀。首先用温水（约60℃）萃取染料，并用tC18柱进行固相萃取净化。沉淀中残留的铝色淀染料用0.02M氢氧化钠萃取。染料色淀中的铝以乙酰丙酮螯合物的形式用乙酰丙酮-乙酸丁酯（1 + 9，v/v）重新萃取到有机层中，并用原子吸收光谱法进行定量。铝色淀的染料部分留在水层中，并以与染料相同的方式进行净化。染料和铝色淀的染料部分在20分钟内通过配有光电二极管阵列检测器的离子对液相色谱法进行定量。每片药中添加10μg每种染料时，染料的回收率为87.0 - 102.2%，每片药中添加50μg每种染料色淀时，染料的回收率为82.9 - 101.6%，靛蓝胭脂红的回收率除外。在40种处方药和非处方药中，有5个样品检测到包装说明书中未标明的染料。在一种药物中发现的最高染料量为1169.5μg赤藓红，在一种抗生素胶囊中检测到。在8种不同剂型的样品中检测到了铝色淀染料。
