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Development and Validation of Ultrahigh-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry Method for Quantitative Determination of Ten Active Compounds in Ge-Gen-Jiao-Tai-Wan 超高效液相色谱-三重四极杆质谱法定量测定葛根胶台丸中10种有效成分的建立与验证
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-10 DOI: 10.1155/2022/4713799
Wenbo Wang, Shuangquan Zhu, Hao Chen, Ning Wu, Han Chen, Dongsheng Wang
A rapid, accurate, and sensitive method for the simultaneous determination of 10 main components, namely puerarin, daidzin, coptisine, epiberberine, jatrorrhizine, berberine, palmatine, coumarin, daidzein, and cinnamic acid in Ge-Gen-Jiao-Tai-Wan, was developed based on ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry. Analysis was performed on an Agilent 1290 Infinity II series UHPLC system, equipped with a Waters ACQUITY UPLC HSS T3 column (100 × 2.1 mm, 1.8 μm) by using (A) 0.1% acetic acid and (B) methanol as mobile phase. The flow rate was 0.3 mL/min, and the injection volume was 1 μL. Mass spectrometry was operated in multiple reaction monitoring mode using an Agilent 6460 triple quadrupole mass spectrometer equipped with an AJS-ESI ion source. Agilent Mass Hunter Work Station Software was employed for data acquisition and processing. All calibration curves showed excellent linear regressions (R2 > 0.9992). The precision, repeatability, and stability of the ten compounds were below 4.56% in terms of relative standard deviation. The average extraction recovery ranged from 96.53% to 102.69% with a relative standard deviation of 1.14–3.78% for all samples. This study potently contributes to the quantitative evaluation of Ge-Gen-Jiao-Tai-Wan, thereby providing a scientific basis for further studies and clinical application of Ge-Gen-Jiao-Tai-Wan.
采用超高效液相色谱-三重四极杆质谱联用技术,建立了葛根胶台丸中葛根素、黄豆苷、黄连碱、小檗碱、小檗碱、棕榈碱、香豆素、大豆苷、肉桂酸等10种主要成分的快速、准确、灵敏的同时测定方法。分析采用Agilent 1290 Infinity II系列UHPLC系统,配备Waters ACQUITY UPLC HSS T3色谱柱(100 × 2.1 mm, 1.8 μm),流动相为(a) 0.1%醋酸,(B)甲醇。流速0.3 mL/min,进样量1 μL。使用配备AJS-ESI离子源的Agilent 6460三重四极杆质谱仪在多反应监测模式下进行质谱分析。采用Agilent Mass Hunter工作站软件进行数据采集和处理。所有校准曲线线性回归良好(R2 > 0.9992)。10个化合物的精密度、重复性和稳定性在相对标准偏差上均小于4.56%。各样品的平均提取回收率为96.53% ~ 102.69%,相对标准偏差为1.14 ~ 3.78%。本研究有力地促进了葛根胶台丸的定量评价,为葛根胶台丸的进一步研究和临床应用提供了科学依据。
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引用次数: 1
A Simple and Sensitive HPLC-MS/MS Assay for the Quantitation of Blonanserin and N-Desethyl Blonanserin in Rat Plasma and Its Application to Pharmacokinetic Study 高效液相色谱-质谱联用法测定大鼠血浆中勃隆霉素和n -去乙基勃隆霉素及其药动学研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-07 DOI: 10.1155/2022/5914581
Shangxu Huang, Xiaoling Li, Zhanzhang Wang, Haoyang Lu, Tao Xiao, Xiao-jia Ni, Shu-jing Liu, Ming Zhang, D. Shang, Y. Wen
A high-performance liquid chromatographic method coupled with triple quadrupole mass spectrometry (LC-MS/MS) for the analysis of blonanserin and its active metabolite, N-desethyl blonanserin, in rat plasma has been developed and validated. The biological samples were treated by simple direct protein precipitation before separation on an Agilent Eclipse Plus C18 column (4.6 × 100 mm, 3.5 μm) with a column temperature of 35°C at a flow rate of 0.5 mL/min. The mobile phase A is a mixture of methanol and water (75 : 25, v/v, 5 mM ammonium formate), and the mobile phase B is acetonitrile containing 0.1% formic acid. The ratio of mobile phase A to mobile phase B is 15 : 85. Electrospray ionization (ESI) multiple reaction monitoring modes are used for detection, which are m/z 368.10 ⟶ 296.90 (blonanserin), m/z 340.15 ⟶ 297.05(N-desethyl blonanserin), and m/z 348.15⟶ 302.05 (N-desethyl blonanserin-d8). The linear response range was 0.1–100.0 ng/mL for blonanserin and N-desethyl blonanserin. The lower limit of quantification (LLOQ), calibration curves, carryover, and matrix effects were sufficiently accurate and precise according to the National Medical Products Administration (NMPA) guidelines for bioanalytical method validation. This analytical method was successfully applied in a blonanserin-poloxamer thermosensitive gel pharmacokinetic study in rats.
建立了一种高效液相色谱-三重四极杆质谱联用(LC-MS/MS)分析大鼠血浆中blonanserin及其活性代谢物n -去乙基blonanserin的方法并进行了验证。分离前,生物样品在Agilent Eclipse Plus C18色谱柱(4.6 × 100 mm, 3.5 μm)上进行简单直接蛋白沉淀处理,柱温为35℃,流速为0.5 mL/min。流动相A为甲醇与水(75:25,v/v, 5mm甲酸铵)的混合物,流动相B为含0.1%甲酸的乙腈。流动相A与流动相B的比例为15:85。采用电喷雾电离(ESI)多反应监测模式进行检测,分别为m/z 368.10 - 296.90 (blonanserin)、m/z 340.15 - 297.05(n-去乙基blonanserin-d8)和m/z 348.15 - 302.05 (n-去乙基blonanserin-d8)。blonanserin和n -去乙基blonanserin的线性响应范围为0.1 ~ 100.0 ng/mL。根据国家药品监督管理局(NMPA)生物分析方法验证指南,定量下限(LLOQ)、校准曲线、结转和基质效应足够准确和精确。该方法成功地应用于勃隆那色林-波洛沙姆热敏凝胶在大鼠体内的药动学研究。
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引用次数: 0
Determination of Glyphosate, Glufosinate, and Their Major Metabolites in Tea Infusions by Dual-Channel Capillary Electrophoresis following Solid-Phase Extraction 固相萃取双通道毛细管电泳法测定茶叶中草甘膦、草铵膦及其主要代谢物
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-04-01 DOI: 10.1155/2022/5687025
M. Nguyen, T. D. Nguyen, M. T. Vu, Hong Anh Duong, H. Pham
In this study, two analytical procedures were developed and validated using dual-channel capillary electrophoresis-coupled contactless conductivity detection (CE-C4D) followed by solid-phase extraction (SPE) for simultaneous determination of glyphosate (GLYP), glufosinate (GLUF), and their two major metabolites, aminomethylphosphonic acid (AMPA) and 3-(methylphosphinico) propionic acid (MPPA), respectively, in a popular beverage such as tea infusions. GLYP, GLUF, and AMPA were analyzed in the first channel using background electrolyte (BGE) of 1 mM histidine (His) adjusted to pH 2.75 by acetic acid (Ace). In contrast, MPPA was quantified in the second channel with a BGE of 30 mM His adjusted to pH 6.7 by 3-(N-morpholino) propanesulfonic acid (MOPS) and 10 µM of cetyltrimethylammonium bromide (CTAB). In addition, the samples of tea infusions were treated using SPE with 10 mL of 0.5 mM HCl in methanol as eluent. At the optimized conditions, the method detection limit (MDL) of GLYP, GLUF, AMPA, and MPPA is 0.80, 1.56, 0.56, and 0.54 μg/l, respectively. The methods were then applied to analyze four target compounds in 16 samples of tea infusions. GLYP was found in two infusion samples of oolong tea with concentrations ranging from 5.34 to 10.74 µg/L, and GLUF was recognized in three samples of green tea infusion in the range of 45.1–53.9 µg/L.
本研究采用双通道毛细管电泳-耦合非接触电导率检测(CE-C4D)和固相萃取(SPE)两种分析方法,建立并验证了两种分析方法,分别用于同时测定茶泡茶等流行饮料中草甘膦(GLYP)、草铵膦(GLUF)及其两种主要代谢物氨甲基膦酸(AMPA)和3-(甲基膦酸)丙酸(MPPA)。GLYP、GLUF和AMPA在第一通道中使用背景电解质(BGE)进行分析,背景电解质为1 mM组氨酸(His),经乙酸(Ace)调节pH为2.75。相比之下,MPPA在第二个通道中定量,BGE为30 mM,用3-(N-morpholino)丙磺酸(MOPS)和10µM十六烷基三甲基溴化铵(CTAB)调节pH为6.7。采用固相萃取法,以10 mL 0.5 mM HCl加入甲醇为洗脱液对茶叶冲剂进行处理。在优化条件下,GLYP、GLUF、AMPA和MPPA的检出限(MDL)分别为0.80、1.56、0.56和0.54 μg/l。然后应用该方法分析了16种茶叶冲剂样品中的4种目标化合物。两种乌龙茶泡茶样品中发现GLYP的浓度范围为5.34 ~ 10.74µg/L,三种绿茶泡茶样品中发现GLUF的浓度范围为45.1 ~ 53.9µg/L。
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引用次数: 4
Home-Made Membraneless Vaporization Gas-Liquid Separator for Colorimetric Determination of Ethanol in Alcoholic Beverages 自制无膜汽化气液分离器比色法测定酒精饮料中乙醇
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-03-31 DOI: 10.1155/2022/7346253
Vanpaseuth Phouthavong, Hayato Inoue, K. Phomkeona, V. Chounlamany
This work utilized the simplicity of a so-called membraneless vaporization (MBL-VP) unit as a gas separator for the colorimetric determination of ethanol in alcoholic beverages. A beverage sample with a volume of 1 mL was directly injected into a small container which was hung from a lid inside a closed 40 mL reused glass bottle without pretreatment such as distillation. An acidified potassium dichromate (Cr2O72−) acceptor solution, preadded to the glass bottle, was reduced to Chromium (III) ion by the diffusion of vaporized ethanol from the sample. After 5 min, the absorbing solution was collected for colorimetric detection at 590 nm. The unit manually quantifies ethanol in the range 1.0–90% (v/v) with satisfactory interday precision but without matrix effect (recovery 89−109%). The method was validated with the conventional distillation/pycnometer method which showed no significant difference of ethanol contents between those two methods and the declared values of 12 alcoholic beverages, indicating sufficient accuracy. Analyses of alcoholic beverages using this method were successful with benefits of simplicity, cheapness, and less energy consumption.
这项工作利用了所谓的无膜汽化(mll - vp)装置作为气体分离器的简单性,用于酒精饮料中乙醇的比色测定。将体积为1ml的饮料样品直接注射到一个小容器中,该小容器挂在一个封闭的40ml重复使用玻璃瓶的盖子上,不进行蒸馏等预处理。酸化的重铬酸钾(Cr2O72−)受体溶液,预先加入到玻璃瓶中,通过从样品中蒸发的乙醇的扩散还原为铬(III)离子。5 min后,收集吸收液在590nm处进行比色检测。该装置手动定量1.0-90% (v/v)范围内的乙醇,日间精密度令人满意,但没有基质效应(回收率89 - 109%)。用常规蒸馏/浓度计法对12种酒精饮料的乙醇含量进行了验证,结果表明两种方法的乙醇含量与申报值无显著差异,具有足够的准确性。使用这种方法对酒精饮料进行分析是成功的,其优点是简单、便宜、耗能少。
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引用次数: 0
Preparation and Photocatalytic Characterization of Modified Nano TiO2/Nd/Rice Husk Ash Material for Rifampicin Removal in Aqueous Solution 纳米TiO2/Nd/稻壳灰改性材料的制备及光催化表征
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-03-30 DOI: 10.1155/2022/2084906
Thuy Dang Thi Ngoc, H. Thi, Dung Nguyen Duc, Sen Nguyen Thi, Toan Nguyen Duc, Nam Nguyen Hoang
Antibiotics like rifampicin are often persistent in the environment. When entering the water, it causes antimicrobial resistance that affects the ecosystem and accumulates in the aquatic organisms and affects human health through the food chain. In this study, titanium dioxide was doped with neodymium (0.01 to 0.8%) using the sol-gel hydrothermal method. TiO2/Nd was then coated on rice husk ash to produce a modified TiO2/Nd/rice husk ash material containing 0.36% (w/w) Nd. The structural characteristics and photocatalytic properties of the materials were analyzed by X-ray diffraction, energy dispersive X-ray, transmission electron microscopy, scanning electron microscopy, forbidden zone energy, and specific surface area. The TiO2/Nd material exhibited a higher photocatalytic decomposition capacity than TiO2 and depended on the Nd content. The rifampicin removal efficiency of TiO2/Nd materials with 0.36 to 0.80% Nd contents was approximately 40% higher than that of TiO2/Nd containing 0.01 to 0.28% Nd. A new photocatalytic TiO2/Nd/rice husk ash material was developed to decompose rifampicin. The rifampicin-degrading efficiency of TiO2/Nd and TiO2/Nd/rice husk ash material reached approximately 86 and 75%, respectively, within 90 min under sunlight. Although a lower efficiency was obtained, the TiO2/Nd/rice husk ash material was selected to degrade rifampicin residue in water via the photocatalytic process (under sunlight) because of its advantages such as requirement of a small amount and easy recovery. In the rifampicin removal process, k values were found to match the zero- and first-order kinetics. In particular, for TiO2/Nd and TiO2/Nd/rice husk ash under solar irradiation, R2 values reached approximately 0.98. These results have been previously published as a preprint.
像利福平这样的抗生素通常会在环境中持续存在。当进入水中时,它会引起抗菌素耐药性,影响生态系统并在水生生物中积累,并通过食物链影响人类健康。本研究采用溶胶-凝胶水热法在二氧化钛中掺杂钕(0.01 ~ 0.8%)。将TiO2/Nd包覆在稻壳灰上,得到Nd含量为0.36% (w/w)的改性TiO2/Nd/稻壳灰材料。采用x射线衍射、能量色散x射线、透射电镜、扫描电镜、禁区能、比表面积等分析了材料的结构特征和光催化性能。TiO2/Nd材料表现出比TiO2更高的光催化分解能力,且与Nd含量有关。Nd含量为0.36 ~ 0.80%的TiO2/Nd材料的利福平去除率比Nd含量为0.01 ~ 0.28%的TiO2/Nd材料高出约40%。研制了一种新型光催化材料TiO2/Nd/稻壳灰分解利福平。TiO2/Nd和TiO2/Nd/稻壳灰材料在光照下90 min内的利福平降解效率分别达到约86%和75%。虽然效率较低,但由于TiO2/Nd/稻壳灰材料用量少、易于回收等优点,采用光催化法(日光下)降解水中利福平残渣。在利福平去除过程中,发现k值符合零级和一级动力学。特别是在太阳辐照下,TiO2/Nd和TiO2/Nd/稻壳灰的R2值约为0.98。这些结果之前已经作为预印本发表过。
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引用次数: 1
Insights into the Aroma Profile of Sauce-Flavor Baijiu by GC-IMS Combined with Multivariate Statistical Analysis GC-IMS结合多元统计分析对酱味白酒香气特征的研究
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-03-29 DOI: 10.1155/2022/4614330
W. Cai, Yurong Wang, Wenping Wang, Na Shu, Q. Hou, F. Tang, Chunhui Shan, Xinquan Yang, Zhuang Guo
Aroma is among the principal quality indicators for evaluating Baijiu. The aroma profiles of sauce-flavor Baijiu produced by 10 different manufacturers were determined by GC-IMS. The results showed that GC-IMS could effectively separate the volatile compounds in Baijiu, and a total of 80 consensus volatile compounds were rapidly detected from all samples, among which 29 volatile compounds were identified, including 5 alcohols, 14 esters, 2 acids, 2 ketones, 5 aldehydes, and 1 furan. According to the differences in aroma profile found by multivariate statistical analysis, these sauce-flavor Baijiu produced by 10 different manufacturers can be further divided into three types. The relative odor activity value of the identified volatile compounds indicated that seven volatile compounds contributed most to the aroma of sauce-flavor Baijiu in order of aroma contribution rate, and they were ethyl hexanoate, ethyl pentanoate, ethyl 2-methylbutanoate, ethyl octanoate (also known as octanoic acid ethyl ester), ethyl 3-methylbutanoate, ethyl butanoate, and ethyl isobutyrate. Correspondingly, the main aromas of these sauce-flavor Baijiu produced by 10 different manufacturers were sweet, fruity, alcoholic, etheral, cognac, rummy, and winey. On the one hand, this study proved that GC-IMS is well adapted to the detection of characteristic volatile aroma compounds and trace compounds in Baijiu, which is of positive significance for improving the aroma fingerprint and database of sauce-flavor Baijiu. On the other hand, it also enriched our knowledge of Baijiu and provided references for the evaluation and regulation of the flavor quality of sauce-flavor Baijiu.
香气是评价白酒质量的主要指标之一。采用气相色谱-液相色谱法测定了10家不同厂家生产的酱味白酒的香气特征。结果表明,GC-IMS能有效分离白酒中的挥发性化合物,在所有样品中快速检出80种一致的挥发性化合物,其中鉴定出29种挥发性化合物,包括5种醇类、14种酯类、2种酸类、2种酮类、5种醛类和1种呋喃。根据多变量统计分析发现的香气特征差异,这10家不同厂家生产的酱味白酒可进一步分为三种类型。经鉴定的挥发性物质的相对气味活性值表明,从香气贡献率排序,对酱味白酒香气贡献最大的挥发性物质为己酸乙酯、戊酸乙酯、2-甲基丁酸乙酯、辛酸乙酯(又称辛酸乙酯)、3-甲基丁酸乙酯、丁酸乙酯和异丁酸乙酯。相应地,这些由10个不同的制造商生产的酱味白酒的主要香气是甜的、果味的、酒精的、醚的、干邑的、拉米的和葡萄酒的。本研究一方面证明了GC-IMS能很好地适应白酒中特征挥发性香气化合物和微量化合物的检测,对完善酱味白酒香气指纹图谱和数据库具有积极意义。另一方面,也丰富了我们对白酒的认识,为酱味白酒风味品质的评价和调控提供了参考。
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引用次数: 15
Quantification of Myoinositol in Serum by Electrochemical Detection with an Unmodified Screen-Printed Carbon Electrode 未经修饰的丝网印刷碳电极电化学检测血清中肌醇含量
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-03-29 DOI: 10.1155/2022/3998338
Xinrui Jin, Yuanqing Zhao, Xiujuan Gu, M. Zhong, Xin Kong, Guangrong Li, Gang Tian, Jinbo Liu
Simple, rapid, and accurate detection of myoinositol (MI) concentration in blood is crucial in diagnosing polycystic ovary syndrome, neurological disorders, and cancer. A novel electrochemical detection (IED) method was established to quantify MI in human serum using a disposable unmodified screen-printed carbon electrode (SPCE) for the first time. MI was detected indirectly by the reaction product of myoinositol dehydrogenase (IDH) and cofactor β-nicotinamide adenine dinucleotide (NAD+). Good linear calibration curves were obtained at the concentration range from 5.0 μM to 500.0 μM (R2 = 0.9981) with the lower limits of detection (LOD) and quantification (LOQ) of 1.0 μM and 2.5 μM, respectively. Recoveries were calculated at three spiked concentrations, and the values were between 90.3 and 106%, with relative standard deviation values of 3.2–6.2% for intraday precision and 7.1–9.0% for interday precision. The SPCE-electrochemical biosensor is simple, accurate, and without modification, showing great potential for point-of-care testing (POCT) of serum MI in clinical samples.
简单、快速、准确地检测血液中肌醇(MI)浓度对诊断多囊卵巢综合征、神经系统疾病和癌症至关重要。首次建立了利用一次性未修饰丝网印刷碳电极(SPCE)定量人血清中心肌梗死的电化学检测方法。通过肌醇脱氢酶(IDH)和辅助因子β-烟酰胺腺嘌呤二核苷酸(NAD+)的反应产物间接检测心肌梗死。在5.0 μM ~ 500.0 μM浓度范围内获得良好的线性校准曲线(R2 = 0.9981),检测下限为1.0 μM,定量限为2.5 μM。加标浓度为90.3 ~ 106%,日内精密度相对标准差为3.2 ~ 6.2%,日内精密度相对标准差为7.1 ~ 9.0%。spce -电化学生物传感器简单、准确、无需修改,在临床样品血清心肌梗死的即时检测(POCT)中显示出巨大的潜力。
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引用次数: 0
Semiconducting Carbon Nanotube-Based Nanodevices for Monitoring the Effects of Chlorphenamine on the Activities of Intracellular Ca2+ Stores 用于监测氯非那明对细胞内Ca2+储存活性影响的半导体碳纳米管纳米器件
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-03-02 DOI: 10.1155/2022/9019262
Viet Anh Pham Ba, Ngoc Pham Van Bach, Thien Nguyen Luong, K. V. Nguyen
We report a flexible and noninvasive method based on field-effect transistors hybridizing semiconducting single-walled carbon nanotubes for monitoring the effects of histamine on Ca2+ release from the intracellular stores of a nonexcitable cell. These nanodevices allowed us to evaluate the real-time electrophysiological activities of HeLa cells under the stimulation of histamine via the recording of the conductance changes of the devices. These changes resulted from the binding of histamine to its receptor type 1 on the HeLa cell membrane. Moreover, the effects of chlorphenamine, an antihistamine, on the electrophysiological activities of a single HeLa cell were also evaluated, indicating that the pretreatment of the cell with chlorpheniramine decreased intracellular Ca2+ release. Significantly, we only utilized a single nanodevice to perform the measurements for multiple cells pretreated with various concentrations of chlorphenamine. This enabled the statistically meaningful analysis of drug effects on cells without errors from device variations. Obtained results indicated the novel advantages of our method such as real-time monitoring and quantitative capability. Our devices, therefore, can be efficient tools for biomedical applications such as electrophysiology research and drug screening.
我们报道了一种基于场效应晶体管杂交半导体单壁碳纳米管的灵活非侵入性方法,用于监测组胺对不可兴奋细胞内Ca2+释放的影响。这些纳米器件使我们能够通过记录器件的电导变化来评估组胺刺激下HeLa细胞的实时电生理活动。这些变化是由于组胺与HeLa细胞膜上的1型受体结合所致。此外,氯苯那敏(一种抗组胺药)对单个HeLa细胞电生理活性的影响也被评估,表明用氯苯那敏预处理细胞可减少细胞内Ca2+释放。值得注意的是,我们仅使用单个纳米器件对不同浓度氯非那明预处理的多个细胞进行测量。这使得对药物对细胞的影响进行统计上有意义的分析,而不会因设备变化而产生误差。结果表明,该方法具有实时监测和定量能力强等优点。因此,我们的设备可以成为电生理学研究和药物筛选等生物医学应用的有效工具。
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引用次数: 2
Quality Evaluation of Decoction Pieces of Gardeniae Fructus Based on Qualitative Analysis of the HPLC Fingerprint and Triple-Q-TOF-MS/MS Combined with Quantitative Analysis of 12 Representative Components 基于HPLC指纹图谱定性分析和三重q - tof -MS/MS结合12种代表性成分定量分析的栀子饮片质量评价
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-02-26 DOI: 10.1155/2022/2219932
Jing Xu, Rongrong Zhou, Lin Luo, Ying Dai, Yaru Feng, Zhihua Dou
In this study, quality evaluation (QE) of 40 batches of decoction pieces of Gardeniae Fructus (GF) produced by different manufacturers of herbal pieces was performed by qualitative analysis of the HPLC fingerprint and ultra-fast liquid chromatography (UFLC)-triple-Q-TOF-MS/MS combined with quantitative analysis of multiple components, which we established previously for QE of traditional medicine. First, HPLC fingerprints of 40 samples were determined, and the common peaks in the reference fingerprint were assigned. Second, the components of the common peaks in the HPLC fingerprints were identified by UFLC-triple-Q-TOF-MS/MS. Finally, the contents of the components confirmed by reference substances were measured. The results showed that there were 28 common peaks in the HPLC fingerprints of 40 samples. The components of these 28 common peaks were identified as 13 iridoids, 4 crocins, 7 monocyclic monoterpenoids, 3 organic acids, and 1 flavonoid. Of these, a total of 12 components, including 7 iridoids of geniposide, shanzhiside, geniposidic acid, deacetyl asperulosidic acid methyl ester, gardenoside, scandoside methyl ester, and genipin gentiobioside, 2 crocins such as crocin I and crocin II, 1 monocyclic monoterpenoid of jasminoside B, 1 organic acid of chlorogenic acid, and 1 flavonoid of rutin, were unambiguously identified by comparison with reference substances. There were certain differences in the contents of these 12 components among 40 samples. The geniposide content ranged from 37.917 to 72.216 mg/g, and the total content of the 7 iridoids ranged from 59.931 to 94.314 mg/g.
本研究采用HPLC指纹图谱和超快速液相色谱(UFLC)-三重q - tof -MS/MS结合多组分定量分析的方法,对不同中药饮片生产厂家生产的40批栀子饮片进行质量评价。首先,对40个样品的HPLC指纹图谱进行了分析,确定了参考指纹图谱中的共有峰;其次,采用UFLC-triple-Q-TOF-MS/MS对指纹图谱中共有峰的成分进行鉴定。最后,测定经对照品确认的组分的含量。结果表明,40份样品的HPLC指纹图谱存在28个共同峰。28个共有峰的成分分别为13个环烯醚萜、4个藏红花素、7个单环单萜类、3个有机酸和1个类黄酮。通过与对照品的比较,共鉴定出京尼平苷、山芝苷、京尼平苷酸、去乙酰曲霉苷酸甲酯、栀子苷、山莨菪苷甲酯、京尼平龙胆苷等7种环烯醚萜类化合物,藏红花素I、藏红花素II等2种藏红花素,茉莉苷B单环单萜类化合物1种,绿原酸有机酸1种,芦丁类黄酮1种。在40个样品中,这12种成分的含量存在一定的差异。栀子苷含量在37.917 ~ 72.216 mg/g之间,7种环烯醚萜类化合物的总含量在59.931 ~ 94.314 mg/g之间。
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引用次数: 3
A Novel Analysis Method for Simultaneous Determination of 31 Pesticides by High-Performance Liquid Chromatography-Tandem Mass Spectrometry in Ginseng 高效液相色谱-串联质谱法同时测定人参中31种农药
IF 2.6 3区 化学 Q3 CHEMISTRY, ANALYTICAL Pub Date : 2022-02-16 DOI: 10.1155/2022/4208243
Xingang Hou, Liangyue Liu, Liping Wei, D. Feng, Meng Lv, Xiumei Wang, X. Yu, Zhongbin Lu, Zhiguang Hou
Ginseng is a perennial herb with a long growth cycle and is known to easily accumulate pesticides during its growth process, seriously threatening people's health. Therefore, to ensure safe consumption, it is necessary to detect and monitor pesticide residues in ginseng. In this study, a novel analysis method was established for simultaneous determination of 31 pesticides in ginseng by high-performance liquid chromatography-mass spectrometry. Ginseng samples were extracted using acetonitrile, cleaned up by primary secondary amine (PSA) solid-phase extraction column eluted with acetonitrile-toluene, and then detected in multiple reaction mode (MRM). The calibration curves of target compounds were linear in the range of 0.005–1.0 mg/L, with correlation coefficients greater than 0.9921. The limits of detection of all the pesticides in ginseng were between 4.4×10−5 and 1.6 × 10−2 mg/kg. For fresh ginseng, the average recoveries ranged from 72.1 to 111.6%, and the relative standard deviations were 1.3–12.2%. For dry ginseng, the average recoveries were 74.3–108.3%, and the relative standard deviations were 0.9–14.9%. The residual concentrations of some pesticides in real samples were greater than the maximum residue limit (MRL) for European Union (EU). The method established here is rapid and simple with high sensitivity and good reproducibility, which is sensitive in the residue analysis of many pesticides in ginseng.
人参是一种多年生草本植物,生长周期长,在生长过程中容易积累农药,严重威胁人们的健康。因此,为了保证人参的安全食用,有必要对人参中的农药残留进行检测和监测。建立了高效液相色谱-质谱联用法同时测定人参中31种农药的分析方法。人参样品用乙腈提取,用乙腈-甲苯洗脱的伯仲胺(PSA)固相萃取柱清洗,然后用多反应模式(MRM)检测。目标化合物在0.005 ~ 1.0 mg/L范围内呈良好的线性关系,相关系数大于0.9921。人参中所有农药的检出限在4.4×10−5 ~ 1.6 ×10−2 mg/kg之间。鲜人参的平均加样回收率为72.1 ~ 111.6%,相对标准偏差为1.3 ~ 12.2%。干参的平均加样回收率为74.3 ~ 108.3%,相对标准偏差为0.9 ~ 14.9%。部分农药在实际样品中的残留浓度大于欧盟规定的最大残留限量。该方法快速简便,灵敏度高,重现性好,可用于人参中多种农药的残留分析。
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引用次数: 5
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Journal of Analytical Methods in Chemistry
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