摘要
建立了高效液相色谱一串联质谱（LC-MS／MS）测定禽蛋中头孢噻肟药物残留的方法。禽蛋样品中的头孢噻肟用纯水提取，乙腈沉淀蛋白，OasisHLB（500mg，6mL）固相萃取柱净化，8mL甲醇洗脱。采用ZorbaxXDB-C18（2．1mm×50mm，3．5μm）色谱柱，以0．2％甲酸水-乙腈为流动相，0．3mL／min梯度洗脱，经高效液相色谱分离后，采用电喷雾质谱正离子模式电离，多反应选择离子检测（MRM）模式测定。检测离子对为m／z456．1／396．1、m／z456．1／324．1，其中m／z456．1／396．1为定量离子对。在1．35～135峭儿范围内标准曲线的线性关系良好，相关系数为0．9993；在1．0、50．0、100μg／kg3个添加水平的平均加标回收率为87％～99％，相对标准偏差为1．9％-3．9％；方法检出限为0．3μg／kg，定量下限为1．0μg／kg。该方法简便、灵敏、准确、可靠，适用于禽蛋中头孢噻肟药物残留的分析。
A confirmative method to determine cefotaxime residue in poultry egg by high performance liquid chromatographytandem mass spectrometry（ HPLC -MS/MS） under multiple reaction monito- ring（MRM） mode was developed. The cefotaxime in sample was extracted with water. Sample prepa- ration involved the protein precipitation with acetonitrile and the clean-up on an Oasis HLB （500 mg, 6 mL） solid phase extraction（SPE） cartridge. The analyte was eluted from the SPE cartridge with 8 mL methanol. The separation of cefotaxime was performed on a Zorbax XDB-C18（2. 1 mm ×50 mm, 3.5μm） column using a mobile phase of 0.2% formic acid（A） - acetonitrile （B） by gradient elution with a flow rate of 0. 3 mL/min. The detection of cefotaxime was carried out by electrospray ionization mass spectrometry under positive mode. The MRM monitored ions, m/z 456. 1/396. 1 and m/z 456. 1/324. 1, were selected as qualitative ions, and m/z 456. 1/396. 1 was selected as quantitative ion. The calibration curve showed a good linearity in the range of 1.35 - 135 μg/L with a correlation coefficient of 0. 999 3. The average spiked recoveries of cefotaxime at three concentration levels of 1.0, 50. 0, 100 μg/kg were between 87% and 99% , and the relative standard deviations（ RSDs, n =6）ranged from 1.9% to 3.9%. The limit of detection（LOD, S/N≥3） and limit of quantification （LOQ, S/N≥10） were 0.3 μg/kg and 1.0 μg/kg, respectively. The results demonstrated that the method was simple, sensitive, accurate and reliable, and was suitable for the determination on cefotaxime residue in poultry egg.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第8期772-776,共5页
Journal of Instrumental Analysis
关键词
头孢噻肟
高效液相色谱
串联质谱
禽蛋
残留
cefotaxime
high performance liquid chromatography（HPLC）
tandem mass spectrometry（MS/MS）
poultry egg
residue
