干旱区生态环境知识资源中心(Arid): 固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物

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	固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物
其他题名	Determination of ten cephalosporins in bee products by solid phase extraction-ultra-performance liquid chromatography-tandem mass spectrometry
	章豪; 吴银良; 张宜文; 许秀琴; 徐峰
来源期刊	色谱
ISSN	1000-8713
出版年	2019
卷号	37 期号:12
中文摘要	建立了蜂产品中10种头孢类药物(头孢喹肟、头孢噻肟、头孢洛宁、头孢哌酮、头孢匹林、头孢氨苄、头孢乙腈、头孢拉定、去乙酰基头孢匹林、头孢唑林)含量的液相色谱-串联质谱测定方法。蜂产品样品中头孢类药物用乙腈-水(80∶20,v/v)溶液提取,离心,上清液经Oasis PRIME HLB固相萃取柱净化,氮吹后复溶,进行液相色谱-串联质谱分析。采用Acquity BEH C18色谱柱,以0.1%(v/v)甲酸水溶液-甲醇体系作为流动相进行梯度洗脱,ESI源正离子模式电离,多反应离子监测模式(MRM)检测,基质校准外标法定量。结果表明,10种头孢类药物在一定浓度范围内峰面积与质量浓度的相关系数(r~2)大于0.999,线性关系良好;检出限为0.15~1.5 mug/kg,定量限为0.50~5.0 mug/kg;在阴性蜂产品样品中的加标回收率为75.0%~89.8%,相对标准偏差(RSD)为1.4%~4.6%(n=5)。该方法检测周期短,准确度和精密度高,能满足多种蜂产品样品中头孢类药物的检测需要。
英文摘要	An ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous quantitative determination of ten cephalosporins in bee products,including honey,royal jelly,and lyophilized royal jelly powder,has been established.The samples were extracted with an acetonitrile-water(80∶20,v/v)solution.After purification by solid phase extraction using an Oasis PRIME HLB cartridge,the extract was blown to dryness under a stream of nitrogen gas and then re-dissolved in 1 mL 0.1%(v/v)formic acid solution and methanol(95∶5,v/v).The samples were separated on an Acquity UPLC BEH C18 column,using a mixture of 0.1%(v/v)formic acid solution and methanol as the mobile phase under gradient elution.The analysis was carried out using a positive electrospray ion source in the multiple reaction monitoring mode.The matrix-matched external standard method was applied to quantitative analysis.Good linear relationships were obtained for the ten cephalosporins in certain concentration ranges,and the correlation coefficients were more than 0.999.The limits of detection and limits of quantification for the ten cephalosporins were in the ranges 0.15-1.5 mug/kg and 0.5-5 mug/kg,respectively.The recoveries for the analytes in the bee products were in the range of 75.0%to 89.8%,with relative standard deviations of 1.4% to 4.6%.This method is characterized by a short analysis time and is suitable for the determination of cephalosporins in different bee products by virtue of its simplicity and reliability.
中文关键词	固相萃取 ; 超高效液相色谱-串联质谱法 ; 头孢类药物 ; 蜂产品
英文关键词	solid phase extraction(SPE) ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) cephalosporins bee products
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6625498
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353258
作者单位	章豪, 宁波市农业科学研究院, 农业农村部农产品质量安全风险评估实验室(宁波), 宁波, 浙江 315040, 中国. 吴银良, 宁波市农业科学研究院, 农业农村部农产品质量安全风险评估实验室(宁波), 宁波, 浙江 315040, 中国. 许秀琴, 宁波市农业科学研究院, 农业农村部农产品质量安全风险评估实验室(宁波), 宁波, 浙江 315040, 中国. 徐峰, 宁波市农业科学研究院, 农业农村部农产品质量安全风险评估实验室(宁波), 宁波, 浙江 315040, 中国. 张宜文, 北京市计量检测科学研究院, 北京 100012, 中国.
推荐引用方式 GB/T 7714	章豪,吴银良,张宜文,等. 固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物[J],2019,37(12).
APA	章豪,吴银良,张宜文,许秀琴,&徐峰.(2019).固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物.色谱,37(12).
MLA	章豪,et al."固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物".色谱 37.12(2019).