Tarbin J A, Clarke P, Shearer G
Ministry of Agriculture, Fisheries and Food, Central Science Laboratory, Sand Hutton, York, UK.
J Chromatogr B Biomed Sci Appl. 1999 Jun 11;729(1-2):127-38. doi: 10.1016/s0378-4347(99)00142-5.
A rapid extraction and clean-up procedure for sulphonamide antibiotics in eggs suitable for both GC-MSD and LC-MS end determinations has been developed. The drugs were extracted using acetonitrile, acidified using acetic acid and cleaned-up using cation- and anion-exchange. For determination by GC-MSD, extracts were derivatised with diazomethane followed by pentafluoropropionic acid anhydride. For LC-MS extracts were taken up in water and used directly. The methodology developed was validated at the 100 and 25 microg kg(-1) levels, equivalent to the MRL and one quarter of the MRL. Results for the GC-MS procedure were quantitated against deuterated sulphadiazine with relative recoveries ranging from 54% for sulphachloropyridazine to 135.5% for sulphamethazine. Recoveries for the LC-MS procedure ranged from 33% for sulphaguanidine to 92% for sulphamethazine and sulphadimethoxine.
已开发出一种适用于气相色谱 - 质谱检测（GC - MSD）和液相色谱 - 质谱检测（LC - MS）的鸡蛋中磺胺类抗生素快速提取和净化程序。药物先用乙腈提取，用乙酸酸化，再通过阳离子和阴离子交换进行净化。对于GC - MSD测定，提取物用重氮甲烷衍生化，然后用五氟丙酸酐衍生化。对于LC - MS，提取物用水溶解后直接使用。所开发的方法在100和25微克/千克水平进行了验证，分别相当于最大残留限量（MRL）和MRL的四分之一。GC - MS程序的结果以氘代磺胺嘧啶进行定量，相对回收率范围从磺胺氯哒嗪的54%到磺胺二甲嘧啶的135.5%。LC - MS程序的回收率范围从磺胺胍的33%到磺胺二甲嘧啶和磺胺间二甲氧嘧啶的92%。
