Larsen E, Egsgaard H, Moller J, With T K
Biomed Mass Spectrom. 1977 Apr;4(2):113-7. doi: 10.1002/bms.1200040211.
Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro-porphyrin permethylester were all found to have the same molecular ion sensitivities as their metal-free porphyrin ester. The relative metalloporphyrin ester content in a sample of porphyrin ester was thus obtained directly as the integrated ion current ratios of the normalized molecular ions. The preparation of calibration samples, including complex formation and the mass spectrometric methodology, is described and discussed.
通过应用积分离子流技术，采用质谱法对具有生物学重要性的卟啉制剂中的金属卟啉污染物进行了定量测定。为此，从一系列含有卟啉酯及其一种金属配合物（已知摩尔比）的校准样品的积分分子离子流比率中，确定了污染金属配合物的相对分子离子灵敏度。发现粪卟啉和尿卟啉全甲酯与铜、锌、铁、钴和镍的二价离子形成的配合物，其分子离子灵敏度与其无金属卟啉酯相同。因此，卟啉酯样品中金属卟啉酯的相对含量可直接作为归一化分子离子的积分离子流比率获得。文中描述并讨论了校准样品的制备，包括配合物的形成和质谱方法。
