CAJ | 학술논문

建立了分散固相萃取-高效液相色谱-串联质谱法( QuEChERS-HPLC-MS/MS)同时测定蜂蜜中吡咯里西啶生物碱(倒千里光、千里光菲林、千里光宁、克氏千里光宁)和异喹啉类生物碱(小檗碱、荷叶碱)的方法。蜂蜜样品经乙腈提取,乙二胺-N-丙基硅烷( PSA)吸附剂净化,HPLC-MS/MS测定。采用Agilent Poroshell 120 SB-C18色谱柱(100 mm ×2.1 mm,2.7μm)分离。以0.1%甲酸溶液和乙腈为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式(MRM)下进行测定,外标法定量。结果表明,在0.1~100μg/L范围内,6种生物碱的相关系数均大于0.99；在1~100μg/kg的添加水平下,所有生物碱回收率均在70%~110%之间；6种生物碱日内精密度小于15%,日间精密度小于20%；方法检出限和定量限分别为0.3和1.0μg/kg。本方法可用于蜂蜜中吡咯里西啶生物碱和异喹啉类生物碱的同时定性和定量分析。
건립료분산고상췌취-고효액상색보-천련질보법( QuEChERS-HPLC-MS/MS)동시측정봉밀중필각리서정생물감(도천리광、천리광비림、천리광저、극씨천리광저)화이규람류생물감(소벽감、하협감)적방법。봉밀양품경을정제취,을이알-N-병기규완( PSA)흡부제정화,HPLC-MS/MS측정。채용Agilent Poroshell 120 SB-C18색보주(100 mm ×2.1 mm,2.7μm)분리。이0.1%갑산용액화을정위류동상진행제도세탈,전분무정리자(ESI+)모식전리,다반응감측모식(MRM)하진행측정,외표법정량。결과표명,재0.1~100μg/L범위내,6충생물감적상관계수균대우0.99；재1~100μg/kg적첨가수평하,소유생물감회수솔균재70%~110%지간；6충생물감일내정밀도소우15%,일간정밀도소우20%；방법검출한화정량한분별위0.3화1.0μg/kg。본방법가용우봉밀중필각리서정생물감화이규람류생물감적동시정성화정량분석。
A method was developed for simultaneous determination of pyrrolizidine alkaloids and isoquinoline alkaloids in honey by dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry ( QuEChERS-HPLC-MS/MS) . The honey samples were extracted with acetonitrile solution and cleaned up with PSA absorbent. Agilent Poroshell 120 SB-C18 chromatographic column was used to separate alkaloids with high sensitivity and satisfactory resolution. The identification and quantification were achieved by using electrospray ionization in positive ion mode ( ESI+) with multiple reaction monitoring (MRM). Matrix-matched calibration curves with good correlation coefficients (R2>0. 99) were obtained in the concentration range of 0. 1-100 μg/L. The recoveries of the spiked samples at 1-100 μg/kg were in the range of 70% to 110% with the RSD of intra-day and inter-day lower than 15% and 20%, respectively. The limits of detection ( LOD) and limits of quantification ( LOQ) for all alkaloids were 0. 3 and 1. 0 μg/kg, respectively. This method was successfully applied to the simultaneous determination of pyrrolizidine alkaloids and isoquinoline alkaloids for quantification and confirmation in honey samples.