柱前衍生-液相色谱-串联质谱法测定红曲中软毛青霉酸含量

伍勋; 施思; 靳祖珑; 沈国芳; 刘宇文

引用本文:	伍勋,施思,靳祖珑,沈国芳,刘宇文.柱前衍生-液相色谱-串联质谱法测定红曲中软毛青霉酸含量[J].中国现代应用药学,2025,42(8):112-116.
	WU XUN,Shi Si,Jin Zulong,Shen Guofang,Liu Yuwen.Determination of puberulic acid content in monascus by Pre-column derivatization-liquid chromatography with tandem mass spectrometry[J].Chin J Mod Appl Pharm(中国现代应用药学),2025,42(8):112-116.

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柱前衍生-液相色谱-串联质谱法测定红曲中软毛青霉酸含量
伍勋¹, 施思¹, 靳祖珑², 沈国芳¹, 刘宇文¹
1.杭州市食品药品检验科学研究院;2.SCIEX中国

摘要:

目的：利用了三甲基硅烷化重氮甲烷对软毛青霉酸进行甲基化衍生,建立红曲中软毛青霉酸高灵敏度检测方法。方法：采用利用超高效液相色谱-三重四极杆质谱对软毛青霉酸两种异构体的甲基化衍生产物进行检测。色谱柱为Phenomenex C8(2.7μm 2.1x100mm),流动相以10mmol.L_-1^甲酸铵为流动相A,50%甲醇水(含有10mmol.L_-1^甲酸铵)为流动相B,梯度洗脱(0～0.5min,A：90%→10%,B：10%→90%,0.5～4min,A：10%, B：90%),流速0.3 mL.min_^-1,柱温40℃,进样量10μL；离子化模式为ESI+,进行多反应监测,选择软毛青霉酸甲基化衍生物(m/z) 255.0→225.0为定量离子,质荷比(m/z)255.0→194.0作为定性离子。结果：对9批红曲样品进行检测,均未检出了软毛青霉酸,合格率100%。结论：所建立的方法经验证,专属性强,可用于红曲中软毛青霉酸成分的检测。

关键词: 红曲软毛青霉酸柱前衍生

DOI：

分类号:R284.1；R917.101

基金项目:中药饮片中真菌毒素检测结果准确性关键因素研究及解决方案

Determination of puberulic acid content in monascus by Pre-column derivatization-liquid chromatography with tandem mass spectrometry

WU XUN¹, Shi Si¹, Jin Zulong², Shen Guofang¹, Liu Yuwen¹

1.Hangzhou Institute for Food and Drug Control;2.SCIEX China

Abstract:

ABSTRACT: OBJECTIVE To establish a highly sensitive detection method for puberulic acid in Monascus by using trimethylsilylated diazomethane for methylation derivation of Penicillic acid. METHODS High performance liquid chromatography triple quadrupole mass spectrometry was used to detect the methylated derivatives of two isomers of puberulic acid. The chromatographic column is Phenomenex C8 (2.7μm,2.1x100mm), and the mobile phase is 10mmol·L-1 ammonium formate as mobile phase A, 50% methanol water (containing 10mmol·L-1 ammonium formate) is used as mobile phase B,Gradient elution (0-0.5min, A: 90%→10%, B: 10%→90%, 0.5-4min, A:10%, B:90%), Flow rate of 0.3 mL·min-1, column temperature 40℃, injection volume 10μL. The ionization mode is ESI+, and multiple reaction monitoring is carried out. The methylated derivative of puberulic acid (m/z) 255.0→225.0 is selected as the quantitative ion, and the mass to charge ratio (m/z) 255.0→194.0 is selected as the qualitative ion. RESULTS Nine batches of monascus samples were tested, and no puberulic acid was detected, with a pass rate of 100%. CONCLUSION The established method has been validated and has strong specificity, and can be used for the detection of puberulic acid in Monascus.

Key words: monascus puberulic acid Pre-column derivatization