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超高压液相色谱-串级质谱分析渔业水中7种激素药物
其他题名Determination of 7 hormones in fisheries water by ultra high-pressure liquid chromatography coupled tandem mass spectrometry
张立坚; 王秀季; 张良滔; 张俊杰; 蔡春
来源期刊分析试验室
ISSN1000-0720
出版年2012
卷号31期号:1页码:58-62
中文摘要建立了同时测定渔业养殖水中氢化可的松、泼尼松、醋酸可的松、睾酮、甲睾酮、黄体酮及苯丙酸诺龙等7种激素残留药物的超高压液相色谱-电喷雾电离串联质谱(UPLC-ESI-MS/MS)分析方法。水样用HLB固相萃取柱净化、浓缩后,洗脱液经氮气吹干,残渣用乙腈-水(V:V=1:1)溶解,以乙腈和0.1%甲酸水溶液为流动相,经ZORBAX SB-C18色谱柱分离后进行LC-MS/MS多反应检测模式作定性定量分析。方法在0.5~40mug/L或1~40mug/L范围具有良好的线性,相关系数大于0.997,检出限(S/N=3)为0.03~0.3mug/L,平均回收率为74.8%~113.0%,相对标准偏差为4.0%~16%。方法适用于渔业养殖水中7种激素的检测分析。
英文摘要An ultra high-pressure liquid chromatography coupled electrospray ionization triple-qudruple tandem mass spectrometric(UHPLC-ESI MS/MS) method has been established for the simultaneous determination of 7 hormones,including cortisone acetate,cortisol,nandrolone prednisone,phenylpropionate,progesterone,Methyltestosterone and testosterone,in fisheries water.The hormones were extracted and cleaned up by an Oasis HLB solid phase extraction cartridge.The extract was evaporated to dryness under nitrogen,and reconstituted in acetonitrile-water(1:1,by volume).The 7 hormones were separated and detected by ZORBAX SB-C18(2.1*50 mm,1.8mum)using 0.1% formic acid(A) and acetonitrile(B) as mobile phase.The target compounds were confirmed and quantified by MS/MS under multiple reaction monitoring(MRM) mode with external standard method.Under the optimal conditions,the calibration curves of 7 hormones showed good linearity with the correlation coefficients >0.997 in the range of 0.5 or 1~40mug/L,the limits of detection(LODs) ranged from 0.03 to 0.3mug/L(S /N = 3),the average recoveries of 7 hormones were in the range 74.8%~113.0%,the relative standard deviations(RSDs) were 4.0%~16%.
中文关键词超高压液相色谱-电喷雾电离质谱 ; 激素 ; 固相萃取 ; 渔业用水
英文关键词Ultra high-pressure liquid chromatography coupled tandem mass spectrometry(UHPLC-MS/MS) Hormones Solid phase extraction(SPE) Fisheries water
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:4435374
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/227936
作者单位广东医学院分析中心, 湛江, 广东 524023, 中国
推荐引用方式
GB/T 7714
张立坚,王秀季,张良滔,等. 超高压液相色谱-串级质谱分析渔业水中7种激素药物[J],2012,31(1):58-62.
APA 张立坚,王秀季,张良滔,张俊杰,&蔡春.(2012).超高压液相色谱-串级质谱分析渔业水中7种激素药物.分析试验室,31(1),58-62.
MLA 张立坚,et al."超高压液相色谱-串级质谱分析渔业水中7种激素药物".分析试验室 31.1(2012):58-62.
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