UPLC-QQQ MS/MS法同时测定松针中的14个成分  

Simultaneous determination of 14 components in pine needles by using UPLC-QQQ MS/MS

作　　者：王信 李彬 辛安琪 王梦凡 马趣环[2] 刘兴国 石晓峰[2] WANG Xin;LI Bin;XIN An-qi;WANG Meng-fan;MA Qu-huan;LIU Xing-guo;SHI Xiao-feng(College of Pharmacy,Gansu University of Traditional Chinese Medicine,Lanzhou 739946,China;Gansu Academy of Medical Sciences,Lanzhou 730000,China;Gansu Institute of Drug Control,Lanzhou 730000,China)

机构地区：[1]甘肃中医药大学药学院,兰州739946 [2]甘肃省医学科学研究院,兰州730000 [3]甘肃省药品检验研究院,兰州730000

出　　处：《药物分析杂志》2024年第10期1713-1721,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：甘肃省科技计划资助项目(23CXGA0038);兰州市科技局指导性项目(2020-ZD-125)。

摘　　要：目的:建立超高效液相色谱串联质谱(UPLC-QQQ MS/MS)同时测定不同品种和产地的松针中14个成分的含量测定方法。方法:运用UPLC-QQQ MS/MS技术,采用Waters ACQUITY UPLC BEH HILIC(100 mm×2.1 mm,1.7μm)色谱柱,柱温35℃,以0.1%的甲酸-乙腈溶液(A)和0.1%的甲酸-水溶液(B)为流动相,梯度洗脱,流速0.2 mL·min^(-1);电喷雾离子源,多反应监测模式。各成分的监测离子对分别为m/z 125.0/79.1(没食子酸)、m/z 105.1/77.2(对羟基苯甲醇)、m/z 109.1/91.1(原儿茶酸)、m/z 93.1/65.2(对羟基苯甲酸)、m/z 190.9/85.2(绿原酸)、m/z 151.8/108.2(香草酸)、m/z 135.1/89.2(咖啡酸)、m/z 167.0/122.9(丁香酸)、m/z 119.2/93.2(对香豆酸)、m/z 208.1/193.0(芥子酸)、m/z 82.0/77.2(苯甲酸)、m/z 91.3/65.3(苯乙酸)、m/z 93.1/65.2(水杨酸)、m/z 103.2/77.2(肉桂酸)。结果:所测定的12份松针样品中各成分含量范围分别为没食子酸0.34~3.42 mg·g^(-1)、对羟基苯甲醇1.32~9.76 mg·g^(-1)、原儿茶酸0~6.32 mg·g^(-1)、对羟基苯甲酸0~19.06 mg·g^(-1)、绿原酸0~18.78 mg·g^(-1)、香草酸0.16~3.81 mg·g^(-1)、咖啡酸0~6.68 mg·g^(-1)、丁香酸0.09~4.64 mg·g^(-1)、对香豆酸0.10~9.90 mg·g^(-1)、芥子酸0.98~19.01 mg·g^(-1)、苯甲酸1.28~18.21 mg·g^(-1)、苯乙酸0.95~20.72 mg·g^(-1)、水杨酸0~3.25 mg·g^(-1)、肉桂酸0~0.27 mg·g^(-1),各成分在测试范围内线性关系良好,平均加样回收率均在98.0%~101.7%,14个成分定量限介于0.01~0.4 ng。结论:本方法适用于常见松针中酚酸类成分的含量测定,其中对羟基苯甲醇、绿原酸、香草酸、丁香酸、对香豆酸、芥子酸、苯甲酸、苯乙酸、水杨酸9个成分为首次在松针中发现和测定,可为松针中多种酚酸类成分含量测定提供参考。Objective:To establish a content determination method for 14 components in pine needles of different varieties and origins simultaneously by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-QQQ MS/MS).Methods:The UPLC-QQQ MS/MS was adopted.A Waters ACQUITY UPLC BEH HILIC(100 mm×2.1 mm,1.7μm)chromatographic column was used,with a column temperature of 35℃.The mobile phase was a mixture of 0.1%formic acid-acetonitrile solution(A)and 0.1%formic acid-aqueous solution(B)for gradient elution,with a flow rate of 0.2 mL·min^(-1).Electrospray ionization was used,and multiple reaction monitoring mode was employed.The monitored ion pairs of each component were m/z 125.0/79.1(gallic acid),m/z 105.1/77.2(p-hydroxybenzyl alcohol),m/z 109.1/91.1(protocatechuic acid),m/z 93.1/65.2(p-hydroxybenzoic acid),m/z 190.9/85.2(chlorogenic acid),m/z 151.8/108.2(vanillic acid),m/z 135.1/89.2(caffeic acid),m/z 167.0/122.9(syringic acid),m/z 119.2/93.2(p-coumaric acid),m/z 208.1/193.0(sinapic acid),m/z 82.0/77.2(benzoic acid),m/z 91.3/65.3(phenylacetic acid),m/z 93.1/65.2(salicylic acid),and m/z 103.2/77.2(cinnamic acid).Results:The content ranges of each component in the 12 determined pine needle samples were as follows:gallic acid 0.34-3.42 mg·g^(-1),p-hydroxybenzyl alcohol 1.32-9.76 mg·g^(-1),protocatechuic acid 0-6.32 mg·g^(-1),p-hydroxybenzoic acid 0-19.06 mg·g^(-1),chlorogenic acid 0-18.78 mg·g^(-1),vanillic acid 0.16-3.81 mg·g^(-1),caffeic acid 0-6.68 mg·g^(-1),syringic acid 0.09-4.64 mg·g^(-1),p-coumaric acid 0.10-9.90 mg·g^(-1),sinapic acid 0.98-19.01 mg·g^(-1),benzoic acid 1.28-18.21 mg·g^(-1),phenylacetic acid 0.95-20.72 mg·g^(-1),salicylic acid 0-3.25 mg·g^(-1),and cinnamic acid 0-0.27 mg·g^(-1).Each component had a good linear relationship within the test range,and the average sample recovery rate was between 98.0%and 101.7%.The quantitative limits of the 14 components were between 0.01 and 0.4 ng.Conclusion:This method is applicable for the determination of phenolic acids in common p

关 键 词：樟子松 油松 华山松 白皮松 雪松 落叶松 酚酸类成分 三重四极杆液质联用 同时测定 

分 类 号：R917[医药卫生—药物分析学]