摘要
目的建立酒和饮料中苯甲酸、山梨酸和脱氢乙酸的超快速液相色谱/电喷雾电离串联质谱(UFLC/ESI-MS/MS)定性鉴别方法。方法酒和饮料样品经提取后采用超快速液相色谱分离,利用优化的电喷雾电离串联质谱(ESI-MS/MS)进行裂解,采用保留时间结合三离子定性原则进行确证。结果在适宜的质谱条件下,电喷雾电离可获得稳定可靠的二级质谱碎片离子,母离子和子离子的关系清晰,苯甲酸的定性离子对为m/z 121→77和m/z 121→59,山梨酸为m/z 111→67和m/z 111→41,脱氢乙酸为m/z 167→83和m/z 167→123。苯甲酸、山梨酸和脱氢乙酸的定量限分别为0.02、0.05和0.02 mg/L。结论该法快速、准确、灵敏,适用于酒和饮料中苯甲酸、山梨酸和脱氢乙酸的确证检测。
Objective To establish a qualitative system for the identification of benzoic acid, sorbic acid and dehydroacetic acid residues in alcoholic drinks and beverages by ultra-fast liquid chromatography coupled with electrospray ionization tandem mass spectrometry （UFLC/ESI-MS/MS）. Methods After the sample was extracted, the separation was performed by UFLC and the cracking was used by the optimized ESI-MS/ MS conditions. Confirmatory detection was carried out by the principle of three qualitative ions and retention time using an UFLC-MS/MS in the negative electrospray ionization mode. Results The MS/MS fragment ions were reliable and steady under the suitable conditions, the cracking ways to the parent ions and fragment ions were clear. Qualitative ion pairs were m/z 121→77 and m/z 121→59 for benzoic acid, m/z 111→~67 and m/z 111→41 for sorbic acid, m/z 167→83 and m/z 167→123 for dehydroaeetie acid. The limits of quantitation （LOQs） were 0.02, 0.05 and 0.02 mg/L for benzoic acid, sorbic acid and dehydroacetic acid, respectively. Conclusion The established method was rapid, accurate and sensitive, it is suitable for confirmation for benzoic acid, sorbic acid and dehydroacetic
出处
《卫生研究》
CAS
CSCD
北大核心
2014年第1期116-120,共5页
Journal of Hygiene Research
基金
浙江省自然科学基金(No.LY12H26003)
宁波市农业与社会发展重大(重点)择优委托项目(No.2011C11021)
关键词
苯甲酸
山梨酸
脱氢乙酸
超快速液相色谱-串联质谱法
定性分析
acid residues in alcoholic drinks benzoic acid, sorbic acid, qualitative analysis and beverages. dehydroacetic acid, UFLC-MS/MS,
