干旱区生态环境知识资源中心(Arid): 高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留

Arid

	高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留
其他题名	Simultaneous determination of seven high risk pesticide residues in royal jelly by high performance liquid chromatography-tandem mass spectrometry
	李樱红 1; 周萍 2; 徐权华 2; 赵焕 2; 邵巧云 2
来源期刊	色谱
ISSN	1000-8713
出版年	2018
卷号	36 期号:2 页码:136-142
中文摘要	建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定蜂王浆中氟胺氰菊酯、三唑醇、蝇毒磷、吡氟乙草灵、多菌灵、乙基硫菌灵和甲基硫菌灵7种高风险农药残留的分析方法.样品在碱性条件下经乙腈提取,无水硫酸钠脱水后,采用HLB固相萃取小柱富集净化.采用Venusil MP C_(18)色谱柱分离,以0.5 mmol/L乙酸铵水溶液(含0.1%(v/v)甲酸)-甲醇(含0.1%(v/v)甲酸)为流动相,梯度洗脱.在电喷雾离子(ESI)源、正离子模式和多反应监测(MRM)模式下采集数据,内标法定量.结果表明,7种高风险农药在5~100 mug/kg范围内线性关系良好,相关系数(r~2)为0.9921~0.9996;方法的检出限和定量限分别为0.5~2.0 mug/kg和1.0~5.0 mug/kg.在高、中、低3个添加水平下7种农药的加标回收率为80.5%~101.3%,相对标准偏差(RSD)为3.6%~9.4%.该法操作简单,灵敏度高,准确可靠,能够满足出口蜂王浆农残限量检测的要求.
英文摘要	A method was developed for the simultaneous determination of seven high risk pesticides in the royal jelly, eg. tau-fluvalinate, triadimenol, coumaphos, haloxyfop, carbendazim, thiophanate-ethyl and thiophanate-methyl by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). First, the royal jelly samples were extracted with acetonitrile under alkaline conditions. After dehydration by anhydrous sodium sulfate, the extracts were enriched and purified through solid-phase extraction (SPE) with Oasis HLB cartridges. Finally, the pesticides were detected by HPLC-MS/MS method. The separation was carried out on a Venusil MP C_(18) column with gradient elution. Methanol (containing 0.1% (v/v) formic acid) and 0.5 mmol/L ammonium acetate aqueous solution (containing 0.1% (v/v) formic acid) were used as the mobile phases. The detection was achieved using electrospray ionization in positive ion (ESI~+) mode and multiple reaction monitoring (MRM) mode for data collection. Quantification was carried out using internal standard method. The results showed that the seven high risk pesticides were linear in the range of 5-100 mug/kg. The linear correlation coefficients (r~2) were 0.9921-0.9996. The limits of detection (LODs) and limits of quantification (LOQs) of the seven high risk pesticides were 0.5-2.0 mug/kg and 1.0-5.0 mug/kg, respectively. The average recoveries at the three spiked levels were 80.5%-101.3%, and the relative standard deviations were 3.6%-9.4% (n=3). This method is simple, effective and sensitive, and is suitable for the determination of the pesticide residues in royal jelly.
中文关键词	高效液相色谱-串联质谱 ; 固相萃取 ; 农药残留 ; 蜂王浆
英文关键词	high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) solid-phase extraction (SPE) pesticide residues royal jelly
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL
WOS研究方向	Chemistry
CSCD记录号	CSCD:6170199
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/238045
作者单位	1.浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国; 2.杭州蜂之语蜂业股份有限公司, 桐庐, 浙江 311500, 中国
推荐引用方式 GB/T 7714	李樱红,周萍,徐权华,等. 高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留[J],2018,36(2):136-142.
APA	李樱红,周萍,徐权华,赵焕,&邵巧云.(2018).高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留.色谱,36(2),136-142.
MLA	李樱红,et al."高效液相色谱-串联质谱法同时测定蜂王浆中7种高风险农药残留".色谱 36.2(2018):136-142.