Journal of Liquid Chromatography & Related Technologies最新文献_第10页

Rapid screening of undeclared hypoglycemics in counterfeit herbal antidiabetic products using HPTLC-MS 利用HPTLC-MS快速筛选假冒中药降糖药中未申报的降糖药

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-05-09 DOI: 10.1080/10826076.2023.2173608

Diva C. Purohit, Jigna Vadalia, H. Joshi, Udaykumar G. Vegad

Abstract Adulterating herbal and dietary supplements with synthetic hypoglycemics is widely practiced, especially in developing and undeveloped countries. A simple, precise, and novel method was developed to simultaneously determine synthetic antidiabetics belonging to different classes, namely biguanide, sulfonylurea, and thiazolidinedione, in counterfeit herbal products as adulterants using HPTLC-MS. The method can simultaneously identify and quantify undeclared synthetic drugs metformin, pioglitazone, glipizide, and glimepiride in herbal as well as dietary supplements. The optimized mobile phase for the TLC system consists of cyclohexane:dichloromethane:1-propanol:saturated solution of ammonium acetate in acetic acid in the ratio of (7:5:2:2, v/v/v/v). The method is highly selective and sensitive for detecting chemicals in complex herbal molecules. Identification and quantification of drugs were performed using the densitometric method. The drugs were confirmed using triple quadrupole mass spectrometry through the MS interface. The screening of market preparations revealed the presence of metformin in two of eight products. This study shows that the method for simultaneous determination of these four drugs can be applied successfully to screen synthetic antidiabetics in the herbal complex matrix as adulterants. Graphical abstract

在草药和膳食补充剂中掺入合成降糖药是一种广泛的做法，特别是在发展中国家和不发达国家。建立了一种简便、准确、新颖的hplc - ms同时测定假药中双胍类、磺脲类和噻唑烷二酮类合成降糖药的方法。该方法可同时鉴别和定量中药及膳食补充剂中未申报的合成药物二甲双胍、吡格列酮、格列吡嗪和格列美脲。TLC系统的优化流动相为环己烷:二氯甲烷:1-丙醇:乙酸铵饱和溶液，比例为(7:5:2:2,v/v/v/v)。该方法对检测复杂草药分子中的化学物质具有高度的选择性和灵敏度。采用密度法对药物进行鉴定和定量。通过质谱界面采用三重四极杆质谱法对药物进行确证。对市场制剂的筛选显示，8种产品中有2种含有二甲双胍。本研究表明，同时测定这四种药物的方法可以成功地用于筛选草药复合基质中合成的抗糖尿病药物作为掺假物。图形抽象

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引用次数: 1

UHPLC-APCI-TQ-MS analytical method to quantify nitrosamine impurities in the commercial formulation of metformin and glipizide UHPLC-APCI-TQ-MS分析方法定量二甲双胍和格列吡嗪市售制剂中亚硝胺类杂质

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-05-09 DOI: 10.1080/10826076.2022.2126856

Ravi Solanki, C. Patel, Ravi Patel, Anujkumar Maradiya, Shalin Parikh, Bhavinkumar Gayakvad

Abstract As per the ICH M7 guideline nitrosamine impurities are referred to as cohort of concern which are having a potential significant carcinogenic risk and for the safe human consumption of drug products, the levels of nitrosamine impurities need to be controlled as per respective permissible daily exposures (PDE). An accurate, precise, sensitive, and robust UPLC-APCI-TQ-MS/MS method has been developed for the quantification of eight nitrosamine impurities in the marketed formulation of metformin and glipizide Tablets. Chromatographic separation was achieved using Kinetex® 150 × 3.0 mm Biphenyl 100 Å, 2.6 µm column with mobile phase A (0.1% w/v formic acid dissolved in water) and mobile phase B (0.1% w/v formic acid dissolved in methanol) with a flow rate of 0.4 mL per minute having run time of 20 min with gradient mode of elution. As per ICH Q2(R1) guideline the method had been validated which demonstrates the sensitivity of the developed method with a good linearity range of 1–5 ng/mL for all eight nitrosamine impurities. The validation parameters suggest that the developed method for the simultaneous quantification of eight nitrosamine impurities in the marketed formulation of metformin hydrochloride and glipizide can be routinely applied in the quality control laboratory. Graphical Abstract

摘要根据ICH M7指南，亚硝胺杂质被称为具有潜在重大致癌风险的关注人群，为了人类安全食用药品，需要根据各自的允许每日暴露量（PDE）控制亚硝胺的杂质水平。已开发出一种准确、准确、灵敏且稳健的UPLC-APCI-TQ-MS/MS方法，用于定量二甲双胍和格列吡嗪片市场配方中的八种亚硝胺杂质。使用Kinetex®150实现色谱分离 × 3 mm联苯100 Å，2.6 µm柱，流动相A（0.1%w/v甲酸溶于水）和流动相B（0.1%w/w甲酸溶于甲醇），流速为0.4 毫升/分钟，运行时间为20 min，采用梯度洗脱模式。根据ICH Q2（R1）指南，该方法已得到验证，证明了所开发方法的灵敏度，线性范围为1-5 所有八种亚硝胺杂质的浓度均为ng/mL。验证参数表明，所开发的同时定量盐酸二甲双胍和格列吡嗪市售制剂中八种亚硝胺杂质的方法可以在质量控制实验室中常规应用。图形摘要

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引用次数: 1

Non-pharmacological interventions for tobacco cessation: A systematic review of existing practices and their effectiveness. 非药物戒烟干预：对现有做法及其有效性的系统回顾。

IF 1 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-03-25 DOI: 10.4081/monaldi.2022.2229

Shyam Kanhaiya Saroj, Tushti Bhardwaj

Smoking tobacco is associated with lung cancer and other life-threatening diseases which requires serious action to curb it. Tobacco cessation interventions are available as pharmacological and non-pharmacological methods or a combination of both. The present review examines the effectiveness of the existing non-pharmacological tobacco cessation interventions and synthesizes the result for the future development of drug-free treatment in the community for tobacco cessation. The literature search was conducted in August 2020, using two electronic databases (PubMed and JSTOR), with search terms: ['tobacco cessation' OR 'smoking cessation'] AND ['intervention'] which included studies published during 2010 and 2020 (till 31st July 2020). All studies were limited to English language, human participants and excluded patients with comorbidities. A total of 2,114 publications were retrieved out of which 11 articles were reviewed. On the basis of intervention used in reviewed studies, we categorized them into seven categories: i. incentive-based intervention, ii. exercise based, iii. telephone-based proactive counselling, iv. mobile phone SMS (Short Message Service) based, v. smartphone app (application) based, vi. web-based intervention, vii. self-help material. Incentives were provided in most of the studies to maintain the retention rate and motivate the participants for completing follow-up. Non-pharmacological interventions for tobacco cessation include a combination of various elements. Our findings suggest that behavioural counselling is one of the most important elements of any non-pharmacological intervention. In addition to behaviour counselling, yoga and exercises along with self-help material, video and phone counselling may have higher efficacy. Thus, practicing non-pharmacological interventions may also increase the cessation rate and reduce the tobacco use burden.

吸烟与肺癌和其他危及生命的疾病有关，因此需要采取严肃的行动加以遏制。戒烟干预措施包括药物和非药物方法，或两者的结合。本综述对现有非药物戒烟干预措施的有效性进行了研究，并对研究结果进行了归纳总结，为今后在社区开展无药物戒烟治疗提供参考。文献检索于 2020 年 8 月进行，使用两个电子数据库（PubMed 和 JSTOR），检索词为['戒烟'或'戒烟']和['干预']，包括 2010 年至 2020 年（截至 2020 年 7 月 31 日）发表的研究。所有研究仅限于英语、人类参与者，并排除了合并症患者。共检索到 2,114 篇文献，其中有 11 篇进行了综述。根据综述研究中使用的干预措施，我们将其分为七类：i.基于激励的干预措施；ii.基于运动的干预措施；iii.基于电话的主动咨询；iv.基于手机短信（SMS）的干预措施；v.基于智能手机应用程序的干预措施；vi.基于网络的干预措施；vii.自助材料。大多数研究都提供了激励措施，以维持保留率并激励参与者完成随访。非药物戒烟干预包括各种因素的组合。我们的研究结果表明，行为咨询是非药物干预中最重要的因素之一。除行为咨询外，瑜伽和运动以及自助材料、视频和电话咨询可能具有更高的疗效。因此，实施非药物干预也可提高戒烟率，减轻烟草使用负担。

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引用次数: 0

Automated online monitoring of lactate and pyruvate in tamoxifen resistant MCF-7 cells using sequential-injection capillary electrophoresis with contactless conductivity detection (SI-CE-C4D) and correlation with MCT1 and MCT4 genes expression 使用顺序注射毛细管电泳非接触式电导检测（SI-CE-C4D）自动在线监测三苯氧胺耐药MCF-7细胞中的乳酸和丙酮酸盐及其与MCT1和MCT4基因表达的相关性

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2098760

Ala A. Alhusban, Lama A. Hamadneh, Aliaa I. Shallan, O. Tarawneh

Abstract Breast cancer is among the most common cancer types worldwide. The first and second line treatment protocols for various stages of breast cancer in females rely on tamoxifen. Until now, the development of tamoxifen resistance is not entirely understood. In this study, an automated sequential injection capillary electrophoresis with capacitively coupled contactless conductivity detector was developed for online levels monitoring of both lactate and pyruvate from the supernatant media of MCF-7 cells developing tamoxifen resistance. Changes in concentration of the two metabolites were simultaneously monitored from three model cell cultures and two control untreated cells. The electrophoretic separation was performed under reversed electroosmotic flow conditions. The system delivers high sample throughput at low sample consumption of 20 µL per analysis. The method is robust and achieved high sensitivity and resolution. Limits of detection were 8.0 and 17.0 nM and linear ranges were 0.15–5 and 0.01–1 mM with a correlation coefficient of 0.9951 and 0.9963 for lactate and pyruvate, respectively. Inter-run and intra-run accuracy were in the range of 95.37–107.02% with precision (RSD, %) of ≤9.84%. The method was completely validated and the data obtained were in agreement with results achieved using the lactate and pyruvate assay kits. The highly informative generated data revealed a significant increase in lactate and pyruvate production in the three tamoxifen resistant MCF-7 cells models compared to the two control cells starting from 5.8 hours and 6.8 hours culturing times, respectively. The increase in concentrations of both lactate and pyruvate were correlated with an increase in MCT1 and MCT4 genes expression. Graphical abstract

摘要癌症是世界上最常见的癌症类型之一。女性癌症不同阶段的一线和二线治疗方案依赖于他莫昔芬。到目前为止，人们还不完全了解三苯氧胺耐药性的发展。在本研究中，开发了一种具有电容耦合非接触式电导率检测器的自动顺序注射毛细管电泳，用于在线监测MCF-7细胞产生三苯氧胺耐药性的上清液培养基中的乳酸和丙酮酸水平。从三个模型细胞培养物和两个对照未处理细胞中同时监测两种代谢物的浓度变化。电泳分离是在反向电渗流条件下进行的。该系统在20的低样本消耗下提供高样本吞吐量每次分析µL。该方法具有较强的鲁棒性，具有较高的灵敏度和分辨率。检测限分别为8.0和17.0 nM和线性范围分别为0.15–5和0.01–1 乳酸和丙酮酸的相关系数分别为0.9951和0.9963。批间和批内准确度在95.37–107.02%之间，精密度（RSD，%）≤9.84%。该方法经过了完全验证，获得的数据与使用乳酸和丙酮酸测定试剂盒获得的结果一致。所产生的信息丰富的数据显示，与两个对照细胞相比，三个三苯氧胺抗性MCF-7细胞模型中的乳酸和丙酮酸产量从5.8开始显著增加小时和6.8 培养时间分别为小时。乳酸盐和丙酮酸盐浓度的增加与MCT1和MCT4基因表达的增加相关。图形摘要

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引用次数: 0

Simultaneous determination of plasma indoles by HPLC with fluorescence detection: Application in polycystic ovary syndrome patients with/without depression 荧光高效液相色谱法同时测定血浆吲哚:在多囊卵巢综合征伴/不伴抑郁患者中的应用

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2124267

Ke Yang, Ying Chen, Zhang Xiaoqing, Q. Zhen, Wenwu Gui, Yanna Ban, Yifan He, Shengnan Pan, Min Ding

Abstract Microbiota-derived indoles were closely associated with psychological disorders like depression. We aimed to develop an HPLC method with fluorescence detection (FLD) for simultaneous determination of plasma indoles, including indoxyl sulfate (3-INDS), indole-3-acetic acid (IAA), indole-3-propionate (IPA), indole (IND) and 3-methylindole (3-MI). Diethyl ether and ethyl acetate were selected as the mixed extractant for the sample preparation. The separation was carried out on a Shim-Pack VP-ODS column (150 × 4.6 mm, 4.6 µm) with the mobile phase composed of 10 mmol/L sodium dihydrogen phosphate/methanol (40:60, v/v). The excitation and emission wavelengths were set at 280 and 355 nm, respectively. The linearities in plasma were obtained in the range of 1.56–400.0 μmol/L for 3-INDS, 0.312–10.0 μmol/L for IAA, 0.125–6.00 μmol/L for IPA, 6.25–400.0 nmol/L for IND, and 1.56–400.0 nmol/L for 3-MI, respectively. The coefficients of variation (CVs) for each analyte of the intra-day and inter-day precisions were within 4.0 and 5.2%, respectively. The recoveries were in the range of 90.1–109.3%. This sensitive and accurate method was applied to analyze plasma indoles for the diagnostic of depression in the patients with polycystic ovary syndrome (PCOS). Graphical Abstract

微生物源性吲哚与抑郁症等心理障碍密切相关。建立了同时测定血浆中吲哚(吲哚-3-乙酸(IAA)、吲哚-3-丙酸(IPA)、吲哚(IND)和3-甲基吲哚(3-MI)的高效液相色谱荧光检测方法。选择乙醚和乙酸乙酯作为混合萃取剂进行样品制备。色谱柱为Shim-Pack VP-ODS (150 × 4.6 mm, 4.6µm)，流动相为10 mmol/L磷酸二氢钠/甲醇(40:60,v/v)。激发波长为280 nm，发射波长为355nm。血浆中3-INDS、IAA、IPA、IND和3-MI的线性范围分别为1.56 ~ 400.0 μmol/L、0.312 ~ 10.0 μmol/L、0.125 ~ 6.00 μmol/L、6.25 ~ 400.0 nmol/L和1.56 ~ 400.0 nmol/L。各分析物的日内、日间精密度变异系数(cv)分别在4.0%和5.2%以内。加样回收率为90.1 ~ 109.3%。该方法灵敏、准确，可用于多囊卵巢综合征(PCOS)患者血浆吲哚含量的分析。图形抽象

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引用次数: 0

Validation and application of a simple and rapid stability-indicating liquid chromatographic assay for the quantification of caffeine from human saliva 快速稳定指示液相色谱法定量人唾液中咖啡因的验证与应用

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2095402

E. Oliphant, Trusha J. Purohit, J. Alsweiler, C. McKinlay, S. Hanning

Abstract A clinical trial is currently underway to examine the efficacy of using caffeine citrate to prevent intermittent hypoxemia in late preterm neonates. Determining caffeine concentration using saliva in this population would be preferable as it is less invasive than plasma sampling, but a suitable method of analysis is required. This paper presents the development and validation of a rapid, efficient and reproducible stability-indicating high-performance liquid chromatography (HPLC) method and extraction protocol for the quantification of caffeine present in saliva. The stability of extemporaneously prepared caffeine citrate solutions (at 20–25 °C) was determined, along with the stability of caffeine spiked saliva samples (at 20–25 and 2–8 °C), to ensure the suitability of the developed method in the analysis of clinical trial samples. Protein precipitation using acetonitrile ensured the complete removal of salivary proteins and resulted in extraction recovery of ≥95% for all samples. The HPLC assay following extraction was linear (R 2>0.99) over the range 0.3–50 µg/mL (lower limit of quantification 0.3 µg/mL). The accuracy of the quality control samples was 94–100% and the relative standard deviation (RSD) was <7% for all samples. Caffeine-spiked saliva samples were stable for three freeze-and-thaw cycles pre-extraction and up to 72 hr post-extraction. The extraction and HPLC methods described were thus suitable for the analysis of clinical trial samples from the Latte Dosage Trial. All caffeine solutions were physically and chemically stable, with concentrations at the end of the three-month test period being within 4% of the baseline concentrations, indicating appropriateness for use as clinical trial medications. Graphical Abstract

目前正在进行一项临床试验，以检查使用枸橼酸咖啡因预防晚期早产儿间歇性低氧血症的有效性。在这一人群中，使用唾液测定咖啡因浓度是可取的，因为它比血浆取样侵入性小，但需要一种合适的分析方法。本文介绍了一种快速、高效、重现性稳定的高效液相色谱(HPLC)定量测定唾液中咖啡因的方法和提取方案。测定临时制备的咖啡因柠檬酸盐溶液(20-25°C)的稳定性，以及咖啡因添加唾液样品(20-25°C和2-8°C)的稳定性，以确保所开发的方法在临床试验样品分析中的适用性。乙腈蛋白沉淀确保了唾液蛋白的完全去除，所有样品的提取回收率≥95%。提取后的HPLC检测在0.3 ~ 50 µg/mL(定量下限0.3 µg/mL)范围内呈线性(r2为0.99)。质量控制样品的准确度为94 ~ 100%，所有样品的相对标准偏差(RSD) <7%。含咖啡因的唾液样品在提取前和提取后的三次冻融循环中都是稳定的。因此，所描述的提取和高效液相色谱方法适用于拿铁剂量试验中临床试验样品的分析。所有的咖啡因溶液在物理和化学上都是稳定的，在三个月的测试期结束时，浓度在基线浓度的4%以内，表明适合用作临床试验药物。图形抽象

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引用次数: 2

Simultaneous determination of nine flavonoids in Farfarae Flos by UHPLC-MS/MS and its application in quality evaluation UHPLC-MS/MS法同时测定法拉中9种黄酮类化合物及其在质量评价中的应用

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2109669

An-Ping Li, Yan-Ping Shi

Abstract Farfarae Flos, a frequently used traditional herbal medicine with outstanding antitussive and anti-asthmatic effects. As an herbal rich in natural flavonoids, the quantitative determination of multi-flavonoids can be helpful to comprehensively evaluate its quality. Herein, an efficient, sensitive and accurate UHPLC-MS/MS method was established to simultaneous determinate nine flavonoids (rutin, hyperin, kaempferol-3-O-rutinoside, hesperidin, luteolin, quercetin, kaempferol, apigenin, and genkwanin) in Farfarae Flos. The calibration curves of the analytes had good linearity (R2 ≥ 0.9991). Limit of detection and limit of quantitation of each analytes was in the range of 1.06 × 10−5–2.26 × 10−3 μg·mL−1 and 3.52 × 10−5–7.53 × 10−3 μg·mL−1. The relative standard deviation (RSD) of the intra-day and inter-day precision was less than 2.71% and 2.94%. The RSD of repeatability test and stability test was less than 2.35% and 2.56%. The recovery rates were in the range of 95.27%–103.60%. The method was further applied to determinate 40 batches of samples that derived from different plant parts and with definite habitat. The results of chemometric statistical analysis showed that, firstly, the content of flavonoids can effectively reflect the differences between traditional medicinal parts and impurities. Secondly, the geographical environment has impact on the quality. In conclusion, this study provides a valuable methodological reference for the quality evaluation and further resource utilization of Farfarae Flos. Graphical Abstract

摘要法法莱是一种常用的中草药，具有显著的镇咳、平喘作用。作为一种富含天然黄酮类化合物的草本植物，多黄酮类化合物含量的定量测定有助于全面评价其质量。本文建立了一种高效、灵敏、准确的超高效液相色谱-质谱联用方法，同时测定法拉中9种黄酮类化合物（芦丁、金丝桃苷、山奈酚-3-O-芸香苷、橙皮苷、木犀草素、槲皮素、山奈奈酚、芹菜素和金瓜素）的含量。分析物的校准曲线具有良好的线性（R2≥0.9991）。每种分析物的检测限和定量限在1.06范围内 × 10−5–2.26 × 10−3 μg·mL−1和3.52 × 10−5–7.53 × 10−3 μg·mL−1。日内和日间精密度的相对标准偏差（RSD）分别小于2.71%和2.94%。重复性试验和稳定性试验的RSD分别小于2.35%和2.56%。回收率在95.27%～103.60%之间。该方法进一步用于测定40批来源于不同植物部位、有明确生境的样品。化学计量统计分析结果表明，黄酮类化合物的含量能够有效地反映中药饮片与杂质的差异。其次，地理环境对质量有影响。总之，本研究为Farfarae Flos的质量评价和进一步的资源利用提供了有价值的方法参考。图形摘要

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引用次数: 0

Identification and characterization of novel hydrolytic degradation products of netarsudil by LC-Q-TOF-MS/MS: In silico toxicity prediction 用LC-Q-TOF-MS/MS鉴定奈沙地尔新型水解降解产物及其在硅毒性预测中的应用

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2022-02-25 DOI: 10.1080/10826076.2022.2089999

Surapuraju Pavan Kumar Raju, Juturu Ravindra Reddy

Abstract A forced degradation study on novel glaucoma drug netarsudil was performed as per ICH and WHO guidelines. All the degradation products were separated from the drug on a C-18 column utilizing ammonium acetate buffer (10 mM, pH 4.90) as a mobile phase-A and acetonitrile: methanol (70:30) v/v as mobile phase-B, by employing gradient elution mode. The injection volume was 10 µL with a 0.8 mL/min flow rate. The detection wavelength was 245 nm and the study was executed at a constant column temperature of 40 °C. Initially, the mass fragmentation pathway of the drug was postulated followed by characterization of degradation products from LC-MS-TOF/MS data. This was followed by LC-MS/TOF studies on the degradation products. Significant degradation was witnessed in alkaline and acidic conditions whereas no signification decline in the drug was observed in other decomposition environments. A total of four degradation products were formed and characterized with the aid of high-resolution mass spectrometry. The mechanistic pathway of formation of all DPs from netarsudil is established. In addition, comparative toxicity properties of the drug and degradation products were established using the online web server Pro Tox II. Graphical Abstract

摘要根据ICH和世界卫生组织指南，对新型青光眼药物耐塔舒地尔进行了强制降解研究。在C-18柱上利用乙酸铵缓冲液（10 mM，pH 4.90）作为流动相a，乙腈∶甲醇（70:30）v/v作为流动相B。注射量为10 µL，0.8 mL/min流速。检测波长245 nm，在40的恒定柱温下进行研究 °C。最初，根据LC-MS-TOF/MS数据对药物的质量裂解途径进行了假设，随后对降解产物进行了表征。随后对降解产物进行LC-MS/TOF研究。在碱性和酸性条件下观察到显著的降解，而在其他分解环境中没有观察到药物的显著下降。共形成四种降解产物，并借助高分辨率质谱进行表征。建立了netarsudil形成所有DP的机制途径。此外，使用在线网络服务器Pro Tox II建立了药物和降解产物的比较毒性特性。图形摘要

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引用次数: 1

Indexation of mixed mode adsorbents using low temperature nitrogen adsorption and Silica-C18 surface energy scale 低温氮吸附和Silica-C18表面能标度对混合模式吸附剂的指数化

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2021-12-14 DOI: 10.1080/10826076.2022.2110117

Dinah Lee, Y. Kazakevich

Abstract Mixed-mode chromatography is becoming increasingly popular in pharmaceutical and biopharmaceutical applications due to its unique selectivity and retention of a variety of compounds. Mixed-mode chromatography is a chromatographic method in which solutes interact with stationary phase through more than one interaction mode or mechanism. It is because of these complex interactions, however, that it is difficult to predict chromatographic behavior of analytes on mixed-mode columns. Characterization of different mixed-mode columns on the basis of surface energy characteristics has not been explored. In this study, different ratios of porous silica (Axia Luna 5 µm Silica – Phenomenex), and C18 (Axia Luna 5 µm C18 – Phenomenex), single mode adsorbents were blended in various ratios and analyzed by Low Temperature Nitrogen Adsorption (LTNA). A variety of commercially available mixed mode columns were also unpacked and the materials were analyzed by LTNA. Adsorption isotherms, surface area, and BET constants were obtained for all the blended materials in various ratios and the mixed-mode materials. A linear relationship between the BET C-constant and the blend ratio of silica has been observed. The results from the commercial mixed mode packing material showed similar surface energy characteristics to single mode C18 materials. This data suggests that the BET C-constant maybe a viable parameter that can be used to characterize mixed-mode columns on the basis of surface energy. Utilizing this surface energy scale in conjunction with the study of retention behaviors on mixed-mode material could lead to improvements in the understanding of method development on mixed-mode columns, allow the comparison of commercialized mixed-mode columns, and even predict retention behavior of an analyte in mixed-mode columns. Graphical Abstract

摘要混合模式色谱法由于其对多种化合物的独特选择性和保留能力，在制药和生物制药应用中越来越受欢迎。混合模式色谱法是溶质通过多种相互作用模式或机理与固定相相互作用的色谱方法。然而，正是由于这些复杂的相互作用，很难预测分析物在混合模式柱上的色谱行为。基于表面能特性的不同混合模式柱的表征尚未得到探索。在本研究中，不同比例的多孔二氧化硅（Axia Luna 5 µm二氧化硅–Phenomenex）和C18（Axia Luna 5 µm C18–Phenomenex），以不同比例混合单模吸附剂，并通过低温氮吸附（LTNA）进行分析。还打开各种市售的混合模式柱的包装，并通过LTNA分析材料。获得了各种比例的所有混合材料和混合模式材料的吸附等温线、表面积和BET常数。已经观察到BET C常数与二氧化硅的共混比之间的线性关系。商业混合模式填料的结果显示出与单模C18材料相似的表面能特性。该数据表明，BET C常数可能是一个可行的参数，可用于基于表面能表征混合模式柱。将这种表面能尺度与对混合模式材料保留行为的研究结合起来，可以提高对混合模式柱方法开发的理解，允许对商业化的混合模式柱进行比较，甚至可以预测分析物在混合模式柱中的保留行为。图形摘要

{"title":"Indexation of mixed mode adsorbents using low temperature nitrogen adsorption and Silica-C18 surface energy scale","authors":"Dinah Lee, Y. Kazakevich","doi":"10.1080/10826076.2022.2110117","DOIUrl":"https://doi.org/10.1080/10826076.2022.2110117","url":null,"abstract":"Abstract Mixed-mode chromatography is becoming increasingly popular in pharmaceutical and biopharmaceutical applications due to its unique selectivity and retention of a variety of compounds. Mixed-mode chromatography is a chromatographic method in which solutes interact with stationary phase through more than one interaction mode or mechanism. It is because of these complex interactions, however, that it is difficult to predict chromatographic behavior of analytes on mixed-mode columns. Characterization of different mixed-mode columns on the basis of surface energy characteristics has not been explored. In this study, different ratios of porous silica (Axia Luna 5 µm Silica – Phenomenex), and C18 (Axia Luna 5 µm C18 – Phenomenex), single mode adsorbents were blended in various ratios and analyzed by Low Temperature Nitrogen Adsorption (LTNA). A variety of commercially available mixed mode columns were also unpacked and the materials were analyzed by LTNA. Adsorption isotherms, surface area, and BET constants were obtained for all the blended materials in various ratios and the mixed-mode materials. A linear relationship between the BET C-constant and the blend ratio of silica has been observed. The results from the commercial mixed mode packing material showed similar surface energy characteristics to single mode C18 materials. This data suggests that the BET C-constant maybe a viable parameter that can be used to characterize mixed-mode columns on the basis of surface energy. Utilizing this surface energy scale in conjunction with the study of retention behaviors on mixed-mode material could lead to improvements in the understanding of method development on mixed-mode columns, allow the comparison of commercialized mixed-mode columns, and even predict retention behavior of an analyte in mixed-mode columns. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"44 1","pages":"880 - 887"},"PeriodicalIF":1.3,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49431578","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Separation optimization and quantitative analysis of phytoestrogens employing reverse-phase high-performance liquid chromatography with UV-VIS detection 紫外可见反相高效液相色谱法优化植物雌激素分离及定量分析

IF 1.3 4区化学 Q4 BIOCHEMICAL RESEARCH METHODS

Journal of Liquid Chromatography & Related Technologies

Pub Date : 2021-12-14 DOI: 10.1080/10826076.2022.2110118

Michael Payette, Marta R. M. Lima, W. M. Coleman, M. Ashraf-Khorassani

Abstract The effect of different acidic modifiers on the separation of seven selected phytoestrogens by reverse-phase high-performance liquid chromatography has been described. Variation in the hydrocarbon chain length of organic acids as represented by acetic acid, propanoic acid, iso-butyric acid, and n-butyric acid as additives to the mobile phase had minimal effect on the separation of phytoestrogens but notably reduced sample turnaround times relative to the turnaround time linked with formic acid. Two different C18 columns were evaluated in attempts of optimize the phytoestrogen separations. Formic acid as a modifier in the mobile phase and an Atlantis C18 column provided the best overall separation at optimum gradient conditions. A higher acid concentration in the mobile phase did not improve the phytoestrogen separation. Higher column temperature (40 °C) provided an improved separation. Finally, the optimized method was used to quantify different phytoestrogens in selected different botanical samples. For this purpose, both internal and external standard methods were compared to obtain the quantitative results. Graphical Abstract

本文介绍了不同酸性改性剂对反相高效液相色谱法分离7种植物雌激素的影响。以乙酸、丙酸、异丁酸和正丁酸为流动相添加剂的有机酸的烃链长度的变化对植物雌激素的分离影响最小，但相对于与甲酸相关的周转时间，样品周转时间显著缩短。为了优化植物雌激素的分离，对两种不同的C18柱进行了评价。在流动相中作为改性剂的甲酸和Atlantis C18柱在最佳梯度条件下提供了最佳的整体分离。流动相中较高的酸浓度并不能改善植物雌激素的分离。较高的柱温度（40 °C）提供了改进的分离。最后，使用优化的方法对所选不同植物样品中的不同植物雌激素进行了定量。为此，对内部和外部标准方法进行了比较，以获得定量结果。图形摘要

{"title":"Separation optimization and quantitative analysis of phytoestrogens employing reverse-phase high-performance liquid chromatography with UV-VIS detection","authors":"Michael Payette, Marta R. M. Lima, W. M. Coleman, M. Ashraf-Khorassani","doi":"10.1080/10826076.2022.2110118","DOIUrl":"https://doi.org/10.1080/10826076.2022.2110118","url":null,"abstract":"Abstract The effect of different acidic modifiers on the separation of seven selected phytoestrogens by reverse-phase high-performance liquid chromatography has been described. Variation in the hydrocarbon chain length of organic acids as represented by acetic acid, propanoic acid, iso-butyric acid, and n-butyric acid as additives to the mobile phase had minimal effect on the separation of phytoestrogens but notably reduced sample turnaround times relative to the turnaround time linked with formic acid. Two different C18 columns were evaluated in attempts of optimize the phytoestrogen separations. Formic acid as a modifier in the mobile phase and an Atlantis C18 column provided the best overall separation at optimum gradient conditions. A higher acid concentration in the mobile phase did not improve the phytoestrogen separation. Higher column temperature (40 °C) provided an improved separation. Finally, the optimized method was used to quantify different phytoestrogens in selected different botanical samples. For this purpose, both internal and external standard methods were compared to obtain the quantitative results. Graphical Abstract","PeriodicalId":16295,"journal":{"name":"Journal of Liquid Chromatography & Related Technologies","volume":"44 1","pages":"888 - 896"},"PeriodicalIF":1.3,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46869503","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1