色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
6期
647-652
,共6页
段永生%王炳玲%艾连峰%郭春海%葛世辉%张婧雯%徐牛生
段永生%王炳玲%艾連峰%郭春海%葛世輝%張婧雯%徐牛生
단영생%왕병령%애련봉%곽춘해%갈세휘%장청문%서우생
在线净化%液相色谱-串联质谱%孕激素%牛奶
在線淨化%液相色譜-串聯質譜%孕激素%牛奶
재선정화%액상색보-천련질보%잉격소%우내
on-line cleanup%liquid chromatography-tandem mass spectrometry(LC-MS/MS)%progesterones%milk
建立了在线净化液相色谱-串联质谱同时测定牛奶中炔诺酮、17α-羟基孕酮、甲羟孕酮、乙酸甲地孕酮、孕酮和醋酸美伦孕酮6种孕激素的方法。本方法采用乙腈为提取溶剂提取目标化合物。提取液经在线净化柱 Cyclone-P净化,经 Phenyl-Hexyl 色谱柱分离,流动相采用0.5%(v / v)甲酸水溶液-乙腈,在电喷雾正离子模式下以多反应监测(MRM)方式测定,内标法定量。方法在0.1~50μg / L 范围内呈线性关系,线性相关系数均大于0.999。6种分析物的测定低限为0.5μg / kg,在牛奶中3个水平的添加回收率在90.8%~107.5%之间,相对标准偏差在6.3%~11.8%之间。该方法快速简便,灵敏度高,选择性好,可用于牛奶样品中孕激素的快速定性定量分析。
建立瞭在線淨化液相色譜-串聯質譜同時測定牛奶中炔諾酮、17α-羥基孕酮、甲羥孕酮、乙痠甲地孕酮、孕酮和醋痠美倫孕酮6種孕激素的方法。本方法採用乙腈為提取溶劑提取目標化閤物。提取液經在線淨化柱 Cyclone-P淨化,經 Phenyl-Hexyl 色譜柱分離,流動相採用0.5%(v / v)甲痠水溶液-乙腈,在電噴霧正離子模式下以多反應鑑測(MRM)方式測定,內標法定量。方法在0.1~50μg / L 範圍內呈線性關繫,線性相關繫數均大于0.999。6種分析物的測定低限為0.5μg / kg,在牛奶中3箇水平的添加迴收率在90.8%~107.5%之間,相對標準偏差在6.3%~11.8%之間。該方法快速簡便,靈敏度高,選擇性好,可用于牛奶樣品中孕激素的快速定性定量分析。
건립료재선정화액상색보-천련질보동시측정우내중결낙동、17α-간기잉동、갑간잉동、을산갑지잉동、잉동화작산미륜잉동6충잉격소적방법。본방법채용을정위제취용제제취목표화합물。제취액경재선정화주 Cyclone-P정화,경 Phenyl-Hexyl 색보주분리,류동상채용0.5%(v / v)갑산수용액-을정,재전분무정리자모식하이다반응감측(MRM)방식측정,내표법정량。방법재0.1~50μg / L 범위내정선성관계,선성상관계수균대우0.999。6충분석물적측정저한위0.5μg / kg,재우내중3개수평적첨가회수솔재90.8%~107.5%지간,상대표준편차재6.3%~11.8%지간。해방법쾌속간편,령민도고,선택성호,가용우우내양품중잉격소적쾌속정성정량분석。
A new method using TurboFlow on-line cleanup liquid chromatography combined with tandem mass spectrometry(MS / MS)has been developed for simultaneous determination of six progesterones including 19-norethindrone,17α-hydroxyprogesterone,medroxyprogester-one,megestrol acetate,progesterone and melengestrol acetate in milk. Samples were extracted by acetonitrile. The analytes in extract were on-line purified directly on Cyclone-P purification column where the sample matrices were washed away. Subsequently,the analytes which were eluted from the extraction column onto Phenyl-Hexyl column were separated with a gradient elution,and detected with electrospray ionization mass spectrometry in the positive scan mode using multiple reaction monitoring( MRM). The isotope internal standards were employed for quantification. As a result,the linearities were satisfactory with the correlation coefficients of﹥0. 999 at concentrations ranging from 0. 1 μg / L to 50 μg / L. Based on the repeated analysis of a known blank sample,the limit of quantification(LOQ)is 0. 5 μg / kg. Average recoveries of the analytes fortified at three levels(1,5 and 25 μg / kg)ranged from 90. 8% to 107. 5% ,and the relative standard deviations(RSDs)ranged from 6. 3% to 11. 8% . This proposed method is sim-ple,rapid,sensitive and highly selective,and can be applied to simultaneous identification and quantification of the six progesterones in milk.