高分离度快速液相色谱-三重串联四极杆质谱快速检查消渴灵片中山麦冬

目的:建立消渴灵片中山麦冬的专属性检测方法.方法:样品经甲醇-氨水超声提取,利用高分离度快速液相色谱-三重串联四极杆质谱(RRLC-QQQ/MS)检测山麦冬.采用Thermo Accla imTM RSLC 120 C18色谱柱(2.1 mm × 100 mm,1.8μm),以乙腈(A)-20 mmol·L-1乙酸铵溶...

Rapid test of Liropes Radix in Xiaokeling tables by rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry

Objective:To establish a method for the specific detection of Liriopes Radix in Xiaokeling tablets.Methods:The samples were extracted by methanol-ammonia,rapid resolution liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry(RRLC-QQQ/MS)was used to detect Liriopes Radix.The Thermo AcclaimTMRSLC 120 C₁₈(2.1 mm×100 mm,1.8μm)column was used.Acetonitrile-20 mmol·L^-1 ammonium acetate solution was used as mobile phase,and gradient elution(0~20 min,5%A→90%A),flow rate was 0.2 m L·min^-1.Column temperature was 30℃,injection was 2μL.The ionized mode was ESI⁺,and m/z723.4→251.2 and m/z 723.4→269.2 were selected as the ion pairs of liriopeside B,and m/z 893.5→463.1 and m/z 893.5→481.2 as the ion pairs of Liriope muscari Baily saponin C,for multi-reaction monitoring.Results:The detection limits of liriopeside B and Liriope muscari Baily saponin C were 0.28μg per tablet and 1.50μg per tablet,respectively.6 batches of samples from batch 111 Xiaokeling tablets were mixed with Liriope spicata var.prolifera Y.T.Ma and Liriope muscari(Decne.)Bailey,4 batches of samples were adulterated with Liriope spicata var.prolifera Y.T.Ma,and 15 batches of samples were adulterated with Liriope muscari(Decne.)Bailey,involving 25 batches of samples from 8 enterprises.Conclusion:The established method is accurate,rapid and simple,which can provide strong technical support for the special treatment of Xiaokeling tablets.