定性和定量分析磺胺氯吡嗪钠可溶性粉中的未知添加物

定性和定量分析了一批兽药磺胺氯吡嗪钠可溶性粉中的未知添加物。使用电位滴定法对该批磺胺氯吡嗪钠可溶性粉进行含量测定,发现滴定异常,根据标准进行的两项鉴别有一项不合格,因此怀疑添加了其他化合物。采用超高效液相色谱-四极杆-飞行时间质谱(UHPLC-Q/TOF MS)对该批样品进行筛查,发现疑似添加物,并使用高效液相色谱-二极管阵列检测(HPLC-DAD)法进行了双重确证和含量测定。该批样品中非法添加物为乙酰甲喹和磺胺二甲嘧啶,添加量分别为40.3和16.4 mg/g。通过总结该批样品非法添加物的发现、确证和含量测定的整个过程,得出一种较好的筛查未知物的模式,为兽药处方外非法添加筛查提供可借鉴的思路。

Qualitative and quantitative analysis of unknown additives in sulfachlorpyrazine sodium soluble powder

A qualitative and quantitative analysis of unknown additives in a batch of veterinary soluble sulfachlorpyrazine sodium powder had been implemented. The content of soluble sulfachlorpyrazine sodium powder was determined by potentiometric titration. The result showed that the titration was aberrant. According to the standard method, one of the two identifications was unqualified. It revealed that some unknown compounds may be doped in the sample. Then the screening of the sample through ultra high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass pectrometry (UHPLC-Q/TOF MS) showed that the suspicious additives were found in the sample. Furthermore, double confirmation and content determination were accomplished by high performance liquid chromatography-diode array detection (HPLC-DAD). Mequindox and sulfadimidine as the illegal additives were detected at 40.3 and 16.4 mg/g respectively. By summarizing the above progress of deduction, validation and content determination, a good pattern was developed for screening illegal additives in veterinary drugs which provided a reference for the inspection of illegal adulterations in veterinary drugs.