Voyksner R D, Tyczkowska K L, Aronson A L
Analytical and Chemical Sciences, Research Triangle Institute, Research Triangle Park, NC 27709.
J Chromatogr. 1991 Jul 5;567(2):389-404. doi: 10.1016/0378-4347(91)80145-3.
Analytical methods for the determination of cloxacillin, ampicillin/hetacillin, and amoxicillin in bovine milk were developed. The methods involved ultrafiltration of milk diluted with methanol, acetonitrile, and water on a 10,000-dalton cut-off filter. Separation of penicillins from other milk components was accomplished by ion-paired chromatography using a microbore column. The penicillins were detected using ultraviolet photodiode array (UV-PDA) detection and confirmed by thermospray liquid chromatography-mass spectrometry (LC-MS). The thermospray spectra of these compounds exhibited [M + H]+ and [M + Na]+ ions along with several fragment ions. The limits of detection for these antibiotics were estimated to be 50 to 100 ppb for LC with UV-PDA detection and 100-200 ppb for thermospray LC-MS detection.
建立了测定牛乳中氯唑西林、氨苄西林/海他西林和阿莫西林的分析方法。这些方法包括在截留分子量为10,000道尔顿的滤膜上，对用甲醇、乙腈和水稀释的牛奶进行超滤。使用微径柱通过离子对色谱法将青霉素与其他牛奶成分分离。采用紫外光电二极管阵列（UV-PDA）检测青霉素，并通过热喷雾液相色谱-质谱联用（LC-MS）进行确证。这些化合物的热喷雾光谱显示出[M + H]+和[M + Na]+离子以及几个碎片离子。这些抗生素的检测限估计为：采用UV-PDA检测的液相色谱法为50至100 ppb，热喷雾LC-MS检测为100 - 200 ppb。
