| 摘要: |
| 定性和定量分析一批兽药硫酸黏菌素可溶性粉中的未知添加物。照《中国兽药典》2010年版一部对该批检品用微生物检定法进行含量测定时,发现该样品的抑菌圈为虚圈,用薄层色谱鉴别该样品,未显示与标准品溶液一致的主斑点,怀疑该样品中有处方外非法添加物。采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q/TOF MS)对该样品进行筛查,发现疑似添加物,并使用液相色谱-二极管阵列检测(HPLC-DAD)法进行了双重确证和含量测定。该样品中非法添加物确证为磺胺氯达嗪和甲氧苄啶,添加量分别为58.5 mg/g和13.4 mg/g。本研究通过建立筛查方法为监管部门提供技术支撑,通过分析非法添加物的可能原因为打击兽药处方外非法添加提供了思路。 |
| 关键词: 硫酸黏菌素可溶性粉 兽药 非法添加物 磺胺氯达嗪 甲氧苄啶 超高效液相色谱-四级杆-飞行时间质谱 液相色谱-二极管阵列检测法 |
| DOI： |
| 投稿时间：2018-02-02修订日期：2018-11-23 |
| 基金项目: |
|
| Qualitative and Quantitative Analysis of Unknown Additives in Colistin Sulphate Soluble Powder byUHPLC-Q/TOF MS and HPLC-DAD |
|
| (Zhejiang Province Institute of Veterinary Drug and Feedstuff) |
| Abstract: |
| A qualitative and quantitative analysis of unknown additives in a batch of colistin sulphate soluble powder had been implemented. During the content determination of the sample with the method of microbiological assay according to Chinese Veterinary Pharmacopoeia 2010, the inhibition zone was virtual. And the thin-layer chromatography (TLC) spots of the sample did not accord with the standard in the identification. The results showed possibility of unknown additives. Suspicious compounds were found by ultra performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q/TOF MS), then double confirmation and content determination were completed by high performance liquid chromatography-diode array detector (HPLC-DAD). The unknown adulterated compounds in this sample were identified as sulfachloropyridazine and trimethoprim with concentration of 58.5 mg/g and 13.4 mg/g, respectively. The research provided technique support for supervisory departments by establishing screening and quantitative method and provided a reference for the fighting illegal adulterations in veterinary drugs by analyzing the possible reasons. |
| Key words: colistin sulphate soluble powder illegal adulteration sulfachloropyridazine trimethoprim ultra performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q/TOF MS) high performance liquid chromatography-diode array detector (HPLC-DAD) |
