Offline two-dimensional liquid chromatography coupled with ion mobility-quadrupole time-of-flight mass spectrometry enabling fourdimensional separation and characterization of the multicomponents from white ginseng and red ginseng

Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensional liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(2 D-LC/IM-QTOF-MS)enabling four-dimensional separations(2 D-LC,IM,and MS),is proposed.In combination with in-house database-driven automated peak annotation,this strategy was utilized to characterize ginsenosides simultaneously from white ginseng(WG)and red ginseng(RG).An offline 2 DLC system configuring an Xbridge Amide column and an HSS T3 column showed orthogonality 0.76 in the resolution of ginsenosides.Ginsenoside analysis was performed by data-independent high-definition MSE(HDMSE)in the negative ESI mode on a Vion?IMS-QTOF hybrid high-resolution mass spectrometer,which could better resolve ginsenosides than MSEand directly give the CCS information.An in-house ginsenoside database recording 504 known ginsenosides and 58 reference compounds,was established to assist the identification of ginsenosides.Streamlined workflows,by applying UNIFI?to automatedly annotate the HDMSEdata,were proposed.We could separate and characterize 323 ginsenosides(including 286 from WG and 306 from RG),and 125 thereof may have not been isolated from the Panax genus.The established 2 D-LC/IM-QTOF-HDMSEapproach could also act as a magnifier to probe differentiated components between WG and RG.Compared with conventional approaches,this dimensionenhanced strategy could better resolve coeluting herbal components and more efficiently,more reliably identify the multicomponents,which,we believe,offers more possibilities for the systematic exposure and confirmative identification of plant metabolites.

Dimension-Enhanced Ultra-High Performance Liquid Chromatography/Ion Mobility-Quadrupole Time-of-Flight Mass Spectrometry Combined with Intelligent Peak Annotation for the Rapid Characterization of the Multiple Components from Seeds of Descurainia sophia

The complex composition of herbal metabolites necessitates the development of powerful analytical techniques aimed to identify the bioactive components.The seeds of Descurainia sophia(SDS)are utilized in China as a cough and asthma relieving agent.Herein,a dimension-enhanced integral approach,by combining ultra-high performance liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(UHPLC/IMQTOF-MS)and intelligent peak annotation,was developed to rapidly characterize the multicomponents from SDS.Good chromatographic separation was achieved within 38 min on a UPLC CSH C18(2.1×100 mm,1.7μm)column which was eluted by 0.1%formic acid in water(water phase)and acetonitrile(organic phase).Collision-induced dissociation-MS^(2)data were acquired by the data-independent high-definition MS^(E)(HDMS^(E))in both the negative and positive electrospray ionization modes.A major components knockout strategy was applied to improve the characterization of those minor ingredients by enhancing the injection volume.Moreover,a self-built chemistry library was established,which could be matched by the UNIFI software enabling automatic peak annotation of the obtained HDMS^(E)data.As a result of applying the intelligent peak annotation workflows and further confirmation process,a total of 53 compounds were identified or tentatively characterized from the SDS,including 29 flavonoids,one uridine derivative,four glucosides,one lignin,one phenolic compound,and 17 others.Notably,four-dimensional information related to the structure(e.g.,retention time,collision cross section,MS^(1)and MS^(2)data)was obtained for each component by the developed integral approach,and the results would greatly benefit the quality control of SDS.

Screening for Plant Toxins in Honey and Herbal Beverage by Ultrahigh-Performance Liquid Chromatography-Ion Mobility-Quadrupole Time of Flight Mass Spectrometry

The standards of plant toxins were separated by a C18 column with gradient elution with 0.1% formic acid/water (V/V) and 0.1% formic acid/acetonitrile (V/V) as mobile phase and acquired by ion mobility-quadrupole time of flight mass spectrometry (IM-QTOF MS) in positive ion mode. A database of 308 plant toxins including retention time, collision cross-section (CCS) and its fragment ions was established. Honey dissolved in water or herbal beverage was extracted by acetonitrile and purified with PSA sorbent, and then acquired by ultrahigh-performance liquid chromatography IM-QTOFMS. The acquired data were processed by comparing with the database we established to confirm the target compounds. The average recoveries for samples at two levels ranged from 60.6% - 120.1%, with relative standard deviation (n = 6) less than 25%. The limit of quantitation for plant toxins ranged from 1 - 20 μg/kg. The developed screening method was used in determination of honey, herbal beverage and honey flavored tea beverage samples. The results showed that berberine was detected in one honey with 1 μg/kg and caffeine was present in some beverages with the concentration from 200 and 5500 μg/kg. This method could meet the requirement for rapid screening of plant toxins in honey and herbal beverage. It can be used for the quality control of honey and herbal beverage in enterprises or quality inspection departments. It also can be used in the rapid screening of food poisoning.

CO₂Absorption Solvent Degradation Compound Identification Using Liquid Chromatography-Mass Spectrometry Quadrapole-Time of Flight (LCMSQTOF)

The degradation of the alkanolamine solvent used in the removal of acid gases from natural gas streams due to exposure to contaminants, thermal degradation and presence of oxygen or oxygen containing compounds will change the solvent properties, such as heat transfer coefficient, diffusion coefficient, and mass transfer coefficient of the solvent. Therefore, characterization and quantification of amine degradation product becomes one of the important analyses to determine alkanolamine solvent’s health. In order to identify degradation products of alkanolamine solvent, analytical strategies by using mass spectrometry (MS) as detector have been studied extensively. In this work, due to the low concentration of the amine degradation product, a method was developed for identification of alkanolamine degradation products using LCMS-QTOF technique. A strategy for identification of trace degradation products has been identified. Six (6) alkanolamine degradation products had been identified by using LCMS-QTOF targeted analysis in the blended alkanolamine solvent used in natural gas processing plant. Another fifteen (15) molecular formulas having similarity in chemical structure to alkanolamine degradation products were identified using untargeted analysis strategy, as possible compounds related to degradation products. Using LCMS-QTOF via targeted and untargeted analysis strategy, without tedious column separation and reference standard, enables laboratory to provide a quick and indicative information for alkanolamine solvent’s organic degradation compounds identification in CO2 adsorption, within reasonable analysis time.

Screening and Identifying of Nephrotoxic Compounds in Lithospermum erythrorhizon Using Live-cell Fluorescence Imaging and Liquid Chromatography Coupled with Tandem Mass Spectrometry

In order to identify the potential nephrotoxic compounds in traditional Chinese medicine Lithospermum erythrorhizon,it was separated into serial fractions according to their polarities.An in vitro method was utilized to determine the nephrotoxicity of these fractions with the help of fluorescence image analysis.As a result,the primary fraction A05 and its secondary fractions C06 ＂C09 and C12 ＂C14 were found to have significant toxicity to LLC-PK1 cell line,as determined by the survive rate less than 20% after they were treated with these fractions.These potential nephrotoxic fractions were further analyzed by multistage and high resolution mass spectrometry.The main compounds in these fractions were tentatively identified to be acetylshikonin,isobutyrylshikonin,β,β＇-dimethyla-cryloylshikonin,and isovalerylshikonin,which may bring nephrotoxicity.

基于UHPLC-Q-TOF-MS/MS技术分析大花萱草花的化学成分

目的采用超高效液相色谱串联四级杆飞行时间质谱对大花萱草花的化学成分进行分析。方法在负离子模式下,采用Waters HSS T3色谱柱,以0.1%甲酸乙腈(A)-0.1%甲酸水(B)为流动相进行梯度洗脱,流速为0.4 ml/min,柱温为35℃,进样量为4μl。建立萱草属化学成分数据库,通过精确的m/z值、特征二级数据、多种数据库和文献中的裂解途径等对化合物进行鉴定。结果共鉴定出59个化合物,包括25个黄酮类、22个苯丙素类、4个脂肪酸类、2个生物碱类以及6个其他类的化合物,其中12个化合物为首次在萱草属植物中发现。结论本方法首次系统、全面、快速地筛选并鉴别大花萱草花中的化合物,为大花萱草花的开发和深入研究提供基础。

UPLC-Q-TOF测定化妆品中9种硝基苯类化合物

建立了超高效液相色谱-四极杆-飞行时间质谱筛查确证化妆品中9种硝基苯类化合物的分析方法。样品经乙酸乙酯提取后,钯碳5%Pd催化氢化,以0.1%(V/V)甲酸水-乙腈为流动相在Poroshell 120 EC-C18(100 mm×4.6 mm,2.7µm)色谱柱上进行梯度洗脱,正离子模式下采用信息依赖性扫描(Auto MS/MS CID)模式采集图谱,以保留时间、一级母离子精确质量数、同位素丰度比、二级子离子精确质量数构建筛查数据库并对检测结果检索,实现化妆品中9种硝基苯类化合物的筛查确证,以分子离子精确质量数提取色谱峰面积定量。结果表明,9种硝基苯类化合物的氢化产物线性关系良好,相关系数(r)大于0.999,方法的检出限为0.01~0.3 mg/kg,定量限为0.04~2.0 mg/kg。膏霜、化妆水、爽身粉、唇膏基质在三个加标水平下的回收率为85.2%~113%,RSD为0.23%~3.61%。该法准确、灵敏、专属性好,适用于化妆品中硝基苯类化合物的筛查和定量分析。

基于UPLC-Q-TOF MS鉴定复方香薷水化学成分

采用超高效液相色谱-四极杆串联飞行时间质谱(UPLC-Q-TOF MS)技术对中药复方香薷水的化学成分进行快速分析鉴定。通过色谱峰响应程度和分离效果优化复方香薷水的前处理方法和仪器条件;采用Agi⁃lent Phe Hex(150 mm×2.1 mm,1.9µm)色谱柱进行分离,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,柱温35℃,流速0.3 mL/min;通过正、负两种离子模式采集复方香薷水的质谱数据,得到精确质量数和二级碎片,结合对照品、Pubchem、安捷伦中药化合物质谱数据库和文献报道等信息对其化合物进行分析鉴定。鉴定出复方香薷水的112个成分,其中黄酮类22个,苯丙素类20个、有机酸18个、萜类14个、生物碱11个、氨基酸5个以及其他类型化合物22个。该研究全面阐述了复方香薷水的化学物质基础,为其质量控制和药效物质研究提供了理论依据。

基于UPLC-Q-TOF-MS和网络药理学探讨黄精糕干预2型糖尿病的作用机制

目的运用超高效液相色谱-四极杆-飞行时间质谱(ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry,UPLC-Q-TOF-MS)和网络药理学,并采用动物实验验证,探讨黄精糕干预2型糖尿病(type 2 diabetes mellitus,T2DM)的作用机制,为产品开发提供依据。方法采用UPLC-Q-TOF-MS分析黄精糕化学成分,网络药理学预测其干预T2DM的作用靶点与通路。将72只大鼠按随机数字表法分为正常组、模型组、二甲双胍组(112.5 mg/kg)及黄精糕低(2.7 g/kg)、中(5.4 g/kg)、高(10.8 g/kg)剂量组,每组12只。1日1次,连续给药30 d。除正常组外,其余大鼠参照保健食品“辅助降血糖功能评价方法”中的方案,采用高脂高糖饮食联合链脲佐菌素(streptozotocin,STZ)诱导T2DM大鼠模型。造模成功后,每隔1周大鼠尾静脉针刺采血测定血糖,末次给药后酶标仪比色法检测血清胰岛素、低密度脂蛋白胆固醇(low density lipoprotein cholesterol,LDL-C)、总胆固醇(total cholesterol,TC)、甘油三酯(triglyceride,TG)、超氧化物歧化酶(superoxide dismutase,SOD)、丙二醛(malondialdehyde,MDA)的含量,ELISA法检测血清胰岛素。结果从黄精糕中鉴定出87个成分和434个作用靶点,与T2DM有160个交集作用靶点。蛋白质-蛋白质相互作用网络图显示,黄精糕可能通过STAT3、SRC、MAPK3、VEGFA、MAPK1等靶点,经AGE-RAGE信号通路干预T2DM。动物实验结果显示,与正常组比较,模型组血清中TC、LDL-C、TG含量及血糖显著升高(P<0.01),血清胰岛素显著降低(P<0.01)。与模型组比较,各给药组血清中LDL-C、TG、TC、MDA含量显著降低(P<0.01),SOD含量显著升高(P<0.01);黄精糕低剂量组血糖降低(P<0.05),黄精糕高剂量组血糖显著降低(P<0.01);黄精糕低剂量组血清胰岛素升高(P<0.05),黄精糕中、高剂量组血清胰岛素含量显著升高(P<0.01)。结论黄精糕可能通过多靶点、多通路干预T2DM。黄精糕具有降血糖、降血脂、抗氧化的作用,可用于辅助治疗T2DM的功能食品开发。

UHPLC-Q-TOF-MS/MS分析青钱柳嫩叶渗漉提取液化学成分

为分析青钱柳嫩叶的化学成分,本研究采取高效液相色谱-四级杆飞行时间串联质谱法(UHPLC-Q-TOFMS/MS)对青钱柳嫩叶渗漉提取液的化学成分进行快速定性分析。在正、负离子模式下全扫描和对母离子电子轰击,根据各化合物的精确分子量及元素组成、主要碎片信息、保留时间以及结合青钱柳相关文献和数据库检索,从青钱柳中共鉴定出94种化合物,包括29种黄酮类、16种三萜类、25种有机酸类、24种其他类化合物。分析结果显示,青钱柳渗漉提取液中含有黄酮、有机酸、三萜、香豆素、氨基酸类等多种化合物,且苹果酸、橙皮素、松脂素、6,7-二羟基香豆素、6-甲基香豆素、5,7-二甲氧基香豆素为首次在青钱柳中发现,本研究结果可为进一步明确青钱柳药效物质基础奠定了基础,为开发青钱柳相关产品提供了理论依据。

基于UHPLC-Q-TOF-MS/MS联合分子网络策略快速分析紫菀中肽类成分

本文建立了超高效液相色谱-四极杆-飞行时间串联质谱(UHPLC-Q-TOF-MS/MS)法联合分子网络策略快速分析紫菀中肽类成分。采用ACQUITY UPLC^(■) HSS T3柱(100 mm×2.1 mm×1.8μm),以乙腈-水为流动相进行梯度洗脱,在正离子模式下,收集紫菀75%乙醇提取物的MS/MS数据,并创建GNPS分子网络。根据标准品、精确相对分子质量、碎片离子等信息,共鉴定出紫菀中43个肽类成分,包括31个环肽类和12个直链肽类,其中分别有16个和8个成分可能为潜在的新型环肽类和直链肽类化合物。UHPLC-Q-TOF-MS/MS联合分子网络策略能够快速、准确、全面地鉴定紫菀中的肽类成分,可为进一步分离紫菀化学成分和研究药效物质基础提供依据。

UPLC-Q-TOF/MS法分析大柴胡汤体内外成分

目的建立超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF/MS)法分析大柴胡汤的体内外成分。方法该药物分析采用Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm);流动相0.1%甲酸-乙腈、0.1%甲酸-水,梯度洗脱;体积流量0.3 mL/min;柱温45℃;电喷雾离子源;正负离子扫描。大鼠灌胃给药3 d后采血,取肝脏、心脏、结肠、肾脏,根据保留时间、精确相对分子质量、一级和二级质谱数据,结合相关对照品、参考文献鉴定血浆和各组织中成分分布。结果共鉴定出60种成分,包括黄酮类33种、蒽醌类7种、酚酸类2种、黄烷醇类1种、类黄酮类1种、异黄酮类1种、香豆素类1种、其他类14种,从大鼠血浆、心脏、肝脏、结肠、肾脏中分别检测到15、5、6、11、7种成分。结论该方法可为大柴胡汤药效物质基础及其作用机制研究提供实验依据。

基于UPLC-Q-TOF-MS技术的脉络宁注射液酯提废渣大孔树脂富集液的化学成分鉴定和含量测定

目的利用超高效液相-四极杆串联飞行时间质谱(UPLC-Q-TOF-MS)技术分析脉络宁注射液酯提废渣的化学成分,为酯提废渣资源的再利用提供科学依据。方法利用ASD-7大孔树脂柱富集脉络宁注射液酯提废渣化学成分,采用UPLC-Q-TOF-MS技术对脉络宁注射液酯提废渣大孔树脂富集液进行数据采集和化学成分鉴定,采用定量软件对绿原酸、异绿原酸、异绿原酸C、灰毡毛忍冬皂苷甲和灰毡毛忍冬皂苷乙进行含量测定。结果共鉴定出脉络宁注射液酯提废渣中42个化学成分,包括9个酚酸类化合物、9个黄酮类化合物、10个环烯醚萜类化合物、8个三萜皂苷类化合物、5个苯丙素类化合物和1个联苄类化合物,定量分析结果显示绿原酸、异绿原酸、异绿原酸C、灰毡毛忍冬皂苷甲和灰毡毛忍冬皂苷乙在考察的浓度范围内与峰面积线性关系良好(r>0.9990),精密度、重复性和稳定性良好,加样回收率为95.38%~103.06%,RSD为0.76%~1.8%。结论本研究可用于脉络宁注射液酯提废渣大孔树脂富集液中化学成分的鉴定以及5种有效成分的准确定量分析,为脉络宁注射液酯提废渣的再利用和制备工艺奠定基础。

基于UPLC-Q-TOF-MS/MS法分析黄花菜的化学成分

目的采用超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF-MS/MS)技术对黄花菜的化学成分进行分析。方法在负离子模式下,采用Waters Atlantis T3色谱柱(4.6 mm×50 mm,5μm),以0.1%甲酸水(A)-乙腈(B)为流动相进行梯度洗脱,流速为0.5 mL·min^(-1),柱温为30℃,进样量为2μL。采用非靶点(NT)、精确靶点(AT)和广泛靶点(ET)法相互结合,全面系统地筛选化合物,进而通过精确的m/z值、特征MS/MS数据、MassBank数据库、PubChem数据库和文献中的裂解途径等对所筛选的化合物进行鉴定。结果共筛选并鉴定出77个化合物,包括39个黄酮类、10个生物碱类、14个多酚类、6个羧酸和8个其他类的化合物,其中27个化合物为首次在萱草属植物中发现。结论本方法可系统、全面、快速地筛选并鉴别黄花菜中的化合物,为黄花菜的产品开发和深入研究提供基础。

GLOBAL ANALYSIS OF THE METABOLITES OF CURCUMIN IN RATS BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPOLE TIME OF-FLIGHT TANDEM MASS SPECTROMETRY

Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after

Analysis of Pharmacodynamic Substance Basis of Fufang Changtai in Treating Colorectal Cancer by UPLC-Q-TOF-MS Combined with Network Pharmacology

[Objectives] To systematically study the main active components of Fufang Changtai(FFCT) in the treatment of colorectal cancer(CRC), and to explore its mechanism of action. [Methods] The main chemical components of FFCT were analyzed by ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) combined with automatic analysis platform, and the main pharmacodynamic substances of FFCT were studied by network pharmacology method and its mechanism of action was explored. The binding degree between the active components and the core targets were verified by molecular docking technology. [Results] A total of 86 compounds were identified from FFCT, among which 26 compounds were Ginsenoside Rg3, Ginsenoside Rb1, Astragaloside III, etc. The key target pathway enrichment analysis showed that FFCT played its role in the treatment of CRC mainly through the PI3K-Akt signaling pathway and MAPK signaling pathway. [Conclusions] This study comprehensively identified the FFCT components. Supplemented by network pharmacology and molecular docking technology, it is expected to provide a scientific theoretical basis and an important reference for FFCT therapeutic components identification, key target verification and mechanism of action in the treatment of CRC.

改进和优化黑果枸杞及其制品中花青素测定的pH示差法

建立一种基于美国官方分析化学师协会(Association of Official Analytical Chemists,AOAC)方法检测黑果枸杞及其制品中花青素含量的改进pH示差法。考察了黑果枸杞及其制品中花青素的最佳提取和检测条件,通过液相色谱-三重四级杆串联质谱法鉴别出黑果枸杞中花青素的具体化学结构,并计算出混合花青素的平均摩尔质量。通过分光光度法测得混合花青素的平均摩尔消光系数,对改进后的pH示差法进行方法学验证和花青素的含量测定。结果显示,最佳提取和检测条件如下:黑果枸杞花青素提取溶剂为盐酸-80%(体积分数)乙醇(3∶97,体积比),料液比为1∶100(g∶mL),提取温度为50℃,提取时间为30 min,缓冲溶液稀释5倍后静置平衡20 min。液相色谱-三重四级杆串联质谱法鉴别黑果枸杞中主要以矮牵牛素类花青素为主(占97.96%),黑果枸杞特有的混合花青素平均摩尔质量为912.7 g/mol,平均摩尔消光系数为29591 L/(mol·cm)。pH示差法改进后能够满足方法学验证要求,固体样品和液体样品最低检出限分别为28.2 mg/100 g、0.282 mg/100 mL。方法改进后花青素提取增长率均大于20%,静置平衡20 min后单次检测结果精密度小于0.3%。以矮牵牛素类花青素代替矢车菊素-3-O-葡萄糖苷计算花青素含量平均提高了2.41倍,能真实地反映黑果枸杞及其制品中花青素的含量。

UPLC-Q-TOF/MS结合化学计量学对不同产地香圆主要成分的研究

建立了超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF/MS)快速分析香圆化学成分的方法。利用UPLC-Q-TOF/MS联用技术,通过一级质谱精确质量数和高分辨二级碎片离子谱图库信息,参照标准品比对及相关文献对化合物结构信息进行鉴定;采用主成分分析(PCA)和正交偏最小二乘判别分析(OPLS-DA)对不同产地香圆样品进行数据分析及质量评价。结果显示:经UPLC-Q-TOF/MS分析指认出29个成分;采自5个产地的25批香圆的PCA和OPLS-DA分析结果一致,样本群处于不同的空间聚落,可以较好地区分且被明显分成了5组,其中广西样品离散性较大,说明同一产地样品的内部差异性较大;安徽、四川、云南、浙江样品分布较为集中;进一步采用VIP值法进行分析,本实验筛选出VIP值>1的8个化学成分作为不同产地香圆差异性的主要化学标记物。所建立的香圆高分辨谱图方法稳定、可靠,可为其质量控制提供参考依据。

复合露酒的非挥发性成分鉴定及抗疲劳效应

该研究采用高效液相色谱-四级杆飞行时间串联质谱联用(HPLC-Q-TOF-MS/MS)法对复合露酒(38%vol)中的非挥发性化合物进行检测,并将复合露酒灌胃至小鼠22 d,考察其对小鼠负重游泳的影响,评价其抗疲劳的保健作用。结果表明,从复合露酒(0.2257 g生药/mL)中共鉴定出52种非挥发性物质,包括皂苷类24种、黄酮类6种、核苷类4种、氨基酸类4种、生物碱类3种、其他11种。与模型组相比,低、中、高剂量组小鼠体质量减少量均极显著减少(P<0.01);中、高剂量组小鼠负重游泳时间均极显著延长(P<0.01);低、中剂量组小鼠血尿素氮(BUN)含量显著增加(P<0.01,P<0.05);低、中、高剂量组小鼠乳酸脱氢酶(LDH)活力、肝糖原(LG)含量显著增加(P<0.01,P<0.05),说明该款复合露酒非挥发性成分丰富,可增强身体对负荷的适应性,具有明显的抗疲劳效果,对功能性食品开发提供一定的基础。

高效液相色谱-串联四极杆质谱法测定荔枝中降糖氨酸A和亚甲基环丙基甘氨酸

建立高效液相色谱-串联四极杆质谱定量分析荔枝中降糖氨酸A和亚甲基环丙基甘氨酸两种降糖氨酸的测定方法。荔枝样品以90%乙醇为提取溶剂进行超声提取,离心取上清,氮吹后用水复溶。经丹磺酰氯衍生化后,采用Waters HSS T3色谱柱(100 mm×2.1 mm,1.8μm)进行分离,柱温为35℃,水(含0.1%甲酸)和乙腈为流动相,梯度洗脱,流量为0.3 mL/min。质谱采用电喷雾电离源,正离子扫描,多反应监测模式进行检测。两种降糖氨酸的质量浓度在0.01~0.50μg/mL范围内与其色谱峰面积线性良好,相关系数均大于0.999,降糖氨酸A的检出限为0.05 mg/kg,亚甲基环丙基甘氨酸的检出限为0.08 mg/kg,加标回收率为81.4%~98.7%,相对标准偏差为3.2%~5.9%(n=6)。该方法操作简单,分析时间短,灵敏度高,准确可靠,为荔枝中降糖氨酸A和亚甲基环丙基甘氨酸两种降糖氨酸的测定提供了有效的技术手段。