超高效液相色谱串联质谱法测定中药类保健品中6种有毒生物碱

Determination of 6 Kinds of Toxic Alkaloids in Health Care Products from Traditional Chinese Medicine Using UPLC-MS/MS

建立了QuEChERS法净化,超高效液相色谱串联三重四极杆质谱法(UPLC-MS/MS)测定中药类保健品中6种有毒生物碱含量的方法。样品以1%甲酸-乙腈超声提取,BEH C18色谱柱(1.7μm,2.1 mm×100 mm)分离,以0.1%甲酸-2 mmol/L乙酸铵的水溶液与含0.1%甲酸的乙腈溶液为流动相梯度洗脱,三重四极杆质谱正离子多反应监测模式检测(MRM),外标法定量。在优化的色谱质谱条件下,6种生物碱在浓度0~20 ng/mL范围内与峰面积线性关系良好,相关系数均大于0.994 2。方法检出限(LOD,S/N=3)为0.002~0.05μg/kg,定量限(LOQ,S/N=10)为0.007~0.15μg/kg,在20、50、100μg/kg的加标浓度下,6种目标分析物的平均回收率为62.3%~98.2%,相对标准偏差(RSD)为1.6%~3.6%。该方法准确、高效、简便,适用于中药类保健品中有毒生物碱的定性、定量筛查。

A method was established for the determination of 6 kinds toxic alkaloids in health care products from traditional Chinese medicine by QuEChERS method and ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with 1% formic acid acetonitrile under ultrasonication,then separated on a BEH C18 column(1.7 μm,2.1 mm×100 mm) by gradient elution,with 0.1% formic acid-2 mmol/L ammonium acetate of aqueous solution and acetonitrile solution containing 0.1% formic acid.The mass spectrometer was operated with positive ionization mode.The analytes were quantified by multiple-reaction monitoring(MRM) with external standards.Under the optimized conditions of chromatography-mass spectrometry,the linear ranges for the six alkaloids were of 0~20 ng/mL,and the correlation coefficients were all greater than 0.994 2,suggesting good linearity of the method.The limit of detection(LOD,S/N=3) and quantification(LOQ,S/N=10) of the method were 0.002~0.05 μg/kg and 0.007~0.15 μg/kg,respectively.At three spiked levels(20,50 and 100 μg/kg),the average recoveries for the target compounds were 62.3%~98.2%,and the relative standard deviation(RSD) were 1.6%~3.6%.The method was accurate,efficient,simple,and suitable for qualitative and quantitative screening of toxic alkaloids in health products from traditional Chinese medicine.