T. Lu, Xiaohong Wang, Qi Zhang, Kun Liu, Tongxin Xu, Quande Wang, Pengfei Zhao, Zhongzhe Cheng
Solasodine, a steroidal alkaloid, is distributed extensively in Solanaceae plants with multiple biological activities such as neuroprotection, antineoplastic and anticonvulsant activities. However, there is little information about the excretion of intact solasodine in vivo. To investigate its excretion, a reliable LC-MS/MS method for quantitation solasodine in rat urine and feces was established and validated. Sample preparation was carried out by liquid-liquid extraction using MTBE as extractant. Moreover, rat urine was preconditioned with BSA, an anti-adsorptive additive, to prevent the nonspecific binding of solasodine to containers and tubes. The method was validated over the range of 4–2000 ng mL−1. The correlation coefficient (r 2) were all above 0.999. The intra- and inter-day precision and accuracy were within 16.9% and between −11.0 and 8.9%, respectively. The recovery of solasodine in urine and feces was in the range of 72.5–80.3 and 75.7–80.2%, respectively. IS-normalized matrix factor ranged from 0.94 to 1.12 with RSD% ≤4.02%. This method was successfully applied to the excretion study of solasodine following oral and intravenous administration.
{"title":"Validated LC-MS/MS method for quantitation of solasodine in rat urine and feces: Blocking nonspecific adsorption","authors":"T. Lu, Xiaohong Wang, Qi Zhang, Kun Liu, Tongxin Xu, Quande Wang, Pengfei Zhao, Zhongzhe Cheng","doi":"10.1556/1326.2022.01079","DOIUrl":"https://doi.org/10.1556/1326.2022.01079","url":null,"abstract":"\u0000 Solasodine, a steroidal alkaloid, is distributed extensively in Solanaceae plants with multiple biological activities such as neuroprotection, antineoplastic and anticonvulsant activities. However, there is little information about the excretion of intact solasodine in vivo. To investigate its excretion, a reliable LC-MS/MS method for quantitation solasodine in rat urine and feces was established and validated. Sample preparation was carried out by liquid-liquid extraction using MTBE as extractant. Moreover, rat urine was preconditioned with BSA, an anti-adsorptive additive, to prevent the nonspecific binding of solasodine to containers and tubes. The method was validated over the range of 4–2000 ng mL−1. The correlation coefficient (r\u0000 2) were all above 0.999. The intra- and inter-day precision and accuracy were within 16.9% and between −11.0 and 8.9%, respectively. The recovery of solasodine in urine and feces was in the range of 72.5–80.3 and 75.7–80.2%, respectively. IS-normalized matrix factor ranged from 0.94 to 1.12 with RSD% ≤4.02%. This method was successfully applied to the excretion study of solasodine following oral and intravenous administration.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41641949","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}
Ning Sun, Zhuo Li, Meng Zhang, Huan He, Libo Zhao, D. Mei, G. Zhu, Xiaoling Wang
In this work, a simple and rapid high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed and validated to carry out the simultaneous measurement of busulfan (BU) and phenytoin (PHT) in the plasma of children. In this method, plasma sample could be prepared by one-step protein precipitation using 1 mL of methanol/water (1:1, v/v). After centrifugation (14,500 rpm, 5 min, 4 °C), 10 μL of the supernatant was injected into a Hypersil Gold C18 column (150 × 2.1 mm, 5 μm, Thermo Fisher Scientific) for separation by gradient elution. Quantification was carried out using multiple reactions monitoring (MRM) under positive scan mode. In the method verification, the calibration curves of BU and PHT showed satisfactory linearity (r > 0.99) at the concentration ranging from 0.02 to 20 μg mL−1. The accuracy and precision were tested at four concentration levels (including the LLOQ level) with the relative error (RE) ranging from −0.80% to 11.45% and coefficient of variation (CV) between 0.93% and 7.74%. There was no pronounced matrix effect to interfere with the quantitative analysis. Compared to determine BU and PHT using two individual methods, less pre-treatment process, labor and blood sample volume are required in this proposed method. Finally, this method was successfully applied to the therapeutic drug monitoring of BU and PHT for children underwent hematological stem cell transplantation.
{"title":"Simultaneously measure the concentrations of busulfan and phenytoin in human plasma using an HPLC-MS/MS method: Application to the TDM for children underwent hematological stem cell transplantation","authors":"Ning Sun, Zhuo Li, Meng Zhang, Huan He, Libo Zhao, D. Mei, G. Zhu, Xiaoling Wang","doi":"10.1556/1326.2022.01069","DOIUrl":"https://doi.org/10.1556/1326.2022.01069","url":null,"abstract":"\u0000 In this work, a simple and rapid high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed and validated to carry out the simultaneous measurement of busulfan (BU) and phenytoin (PHT) in the plasma of children. In this method, plasma sample could be prepared by one-step protein precipitation using 1 mL of methanol/water (1:1, v/v). After centrifugation (14,500 rpm, 5 min, 4 °C), 10 μL of the supernatant was injected into a Hypersil Gold C18 column (150 × 2.1 mm, 5 μm, Thermo Fisher Scientific) for separation by gradient elution. Quantification was carried out using multiple reactions monitoring (MRM) under positive scan mode. In the method verification, the calibration curves of BU and PHT showed satisfactory linearity (r > 0.99) at the concentration ranging from 0.02 to 20 μg mL−1. The accuracy and precision were tested at four concentration levels (including the LLOQ level) with the relative error (RE) ranging from −0.80% to 11.45% and coefficient of variation (CV) between 0.93% and 7.74%. There was no pronounced matrix effect to interfere with the quantitative analysis. Compared to determine BU and PHT using two individual methods, less pre-treatment process, labor and blood sample volume are required in this proposed method. Finally, this method was successfully applied to the therapeutic drug monitoring of BU and PHT for children underwent hematological stem cell transplantation.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67652884","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}
A new pretreatment method termed ultrasound-assisted extraction (UAE) which is combined with solid-phase extraction which is combined with dispersive liquid-liquid microextraction (SPE-DLLME) followed by gas chromatography-flame ionization detector (GC-FID) analysis has been developed for the determination of diazinon in garden parsley as vegetable samples. The analyte was extracted from garden parsley sample using ultrasound-assisted extraction followed by solid-phase extraction followed by dispersive liquid-liquid microextraction. Various parameters that affect the efficiency of the extraction techniques have been optimized. The calibration plot was linear in the range of 5.0–1,000 μg kg−1 with detection limit of 1.0 μg kg−1 for diazinon in garden parsley samples. The results confirm the suitability of the UAE-SPE-DLLME-GC-FID as a sensitive method for the analysis of the targeted analyte in garden parsley samples.
{"title":"Development of ultrasound-assisted extraction followed by solid-phase extraction followed by dispersive liquid–liquid microextraction followed by gas chromatography for the sensitive determination of diazinon in garden parsley as vegetable samples","authors":"M. Rezaee, F. Khalilian, M. Pourjavid","doi":"10.1556/1326.2022.01086","DOIUrl":"https://doi.org/10.1556/1326.2022.01086","url":null,"abstract":"\u0000 A new pretreatment method termed ultrasound-assisted extraction (UAE) which is combined with solid-phase extraction which is combined with dispersive liquid-liquid microextraction (SPE-DLLME) followed by gas chromatography-flame ionization detector (GC-FID) analysis has been developed for the determination of diazinon in garden parsley as vegetable samples. The analyte was extracted from garden parsley sample using ultrasound-assisted extraction followed by solid-phase extraction followed by dispersive liquid-liquid microextraction. Various parameters that affect the efficiency of the extraction techniques have been optimized. The calibration plot was linear in the range of 5.0–1,000 μg kg−1 with detection limit of 1.0 μg kg−1 for diazinon in garden parsley samples. The results confirm the suitability of the UAE-SPE-DLLME-GC-FID as a sensitive method for the analysis of the targeted analyte in garden parsley samples.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41896429","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}
Fuke Yangrong pill, a traditional Chinese patent medicine, with the functions of nourishing qi and blood, soothing liver and relieving depression, regulating menstruation and removing blood stasis, is composed of 16 Chinese medicinal herbs. For quality control purpose, an HPLC method was established for simultaneous quantification of paeoniflorin, hesperidin and ligustilide in Fuke Yangrong pill. With acetonitrile-0.1% formic acid as mobile phase, gradient elution was carried out using Agilent ZORBAX Eclipse Plus C18 column (250 mm × 4.6 mm, 5.0 μm) at 1.0 mL min−1. Detection wavelength was set at 230 nm for paeoniflorin, 280 nm for hesperidin and ligustilide. The temperature was 30 °C. There was a good linearity between the peak area and the concentration of each component to be measured within their linear range (r ≥ 0.9994). The average recoveries were between 98.6% and 102.6% with RSDs no more than 2.93%. This method was validated to be accurate and convenient, which is suitable for the quality control of Fuke Yangrong pill.
福科养荣丸是一种传统的中成药，具有滋补气血、疏肝解郁、调经化瘀的功效，由16种中草药组成。为控制质量，建立了同时测定妇科养荣丸中芍药苷、橙皮苷和藁本内酯含量的高效液相色谱法。以乙腈-0.1%甲酸为流动相，采用Agilent ZORBAX Eclipse Plus C18色谱柱(250 mm × 4.6 mm, 5.0 μm)，流速1.0 mL min - 1梯度洗脱。芍药苷的检测波长为230 nm，橙皮苷和藁本内酯的检测波长为280 nm。温度是30°C。峰面积与各待测成分浓度在线性范围内呈良好的线性关系(r≥0.9994)。平均加样回收率为98.6% ~ 102.6%，rsd≤2.93%。结果表明，该方法准确、简便，适用于妇科养荣丸的质量控制。
{"title":"Simultaneous determination of multiple components in Fuke Yangrong pill by HPLC","authors":"Hua Wang, Changjuan Zhan, Yi Wang","doi":"10.1556/1326.2022.01081","DOIUrl":"https://doi.org/10.1556/1326.2022.01081","url":null,"abstract":"\u0000 Fuke Yangrong pill, a traditional Chinese patent medicine, with the functions of nourishing qi and blood, soothing liver and relieving depression, regulating menstruation and removing blood stasis, is composed of 16 Chinese medicinal herbs. For quality control purpose, an HPLC method was established for simultaneous quantification of paeoniflorin, hesperidin and ligustilide in Fuke Yangrong pill. With acetonitrile-0.1% formic acid as mobile phase, gradient elution was carried out using Agilent ZORBAX Eclipse Plus C18 column (250 mm × 4.6 mm, 5.0 μm) at 1.0 mL min−1. Detection wavelength was set at 230 nm for paeoniflorin, 280 nm for hesperidin and ligustilide. The temperature was 30 °C. There was a good linearity between the peak area and the concentration of each component to be measured within their linear range (r ≥ 0.9994). The average recoveries were between 98.6% and 102.6% with RSDs no more than 2.93%. This method was validated to be accurate and convenient, which is suitable for the quality control of Fuke Yangrong pill.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41818780","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}
In this study, an accurate, simple, economical and precise Reversed-Phase High Pressure Liquid Chromatography (RP-HPLC) method was developed for the simultaneous estimation of Ozenoxacin and Benzoic Acid in a pharmaceutical cream formulation, according to the International Conference on Harmonisation (ICH) guidelines. Chromatographic separation was achieved by gradient elution, on RP-HPLC Instrument, equipped with column C8 (150 mm × 4.6 mm, 5 μm particle size) using Ultra Violet (UV) detector at 235 nm wavelength, by using Mobile Phase A: triethylamine, trifloroacetic acid and water (1:1:1000) and Mobile Phase B: methanol and Diluent: water, acetonitrile and triethylamine (500:500:1), at flow rate 0.8 mL min−1; injection volume of 20 μL; column oven temperature 45 °C and sample temperature: 25 °C; Run time: 15 min. All the validation parameters were within the acceptance criteria, as per ICH requirements, for Ozenoxacin and Benzoic acid. Consequently, this method has found to be validated, simple, rapid and successfully applicable, to the simultaneous estimation of Ozenoxacin and Benzoic acid by RP-HPLC, for routine analytical testing in quality control, with a run time of 15 min and for future research studies. Forced degradation of Ozenoxacin cream 1% w/w formulation was performed and found that validated method has stability indicating potential that needs to be further studied.
在本研究中，根据国际协调会议(ICH)的指导方针，建立了一种准确、简单、经济、精确的反相高压液相色谱(RP-HPLC)方法，用于同时估计药物乳膏制剂中奥硝沙星和苯甲酸的含量。色谱分离采用梯度洗脱，在反相高效液相色谱仪上，柱为C8 (150 mm × 4.6 mm, 5 μm粒径)，紫外检测器，波长235 nm，流动相A:三乙胺、三氟乙酸和水(1:1:1000)，流动相B:甲醇和稀释剂:水、乙腈和三乙胺(500:500:1)，流速0.8 mL min−1;注射量20 μL;柱箱温度45℃，样品温度25℃;片长:15分钟。根据ICH要求，所有验证参数均在奥唑诺星和苯甲酸的验收标准范围内。结果表明，该方法简便、快速，可用于反相高效液相色谱法同时测定奥硝沙星和苯甲酸的含量，可用于常规的质量控制分析检测，运行时间为15 min，可用于后续的研究。对1% w/w配方的奥硝沙星乳膏进行强制降解，发现验证方法具有稳定性，表明有进一步研究的潜力。
{"title":"Analytical method validation on simultaneous estimation of Ozenoxacin and Benzoic acid in pharmaceutical formulation","authors":"Amarnath Reddy Ramireddy, D. K. Behara","doi":"10.1556/1326.2022.01064","DOIUrl":"https://doi.org/10.1556/1326.2022.01064","url":null,"abstract":"\u0000 In this study, an accurate, simple, economical and precise Reversed-Phase High Pressure Liquid Chromatography (RP-HPLC) method was developed for the simultaneous estimation of Ozenoxacin and Benzoic Acid in a pharmaceutical cream formulation, according to the International Conference on Harmonisation (ICH) guidelines. Chromatographic separation was achieved by gradient elution, on RP-HPLC Instrument, equipped with column C8 (150 mm × 4.6 mm, 5 μm particle size) using Ultra Violet (UV) detector at 235 nm wavelength, by using Mobile Phase A: triethylamine, trifloroacetic acid and water (1:1:1000) and Mobile Phase B: methanol and Diluent: water, acetonitrile and triethylamine (500:500:1), at flow rate 0.8 mL min−1; injection volume of 20 μL; column oven temperature 45 °C and sample temperature: 25 °C; Run time: 15 min. All the validation parameters were within the acceptance criteria, as per ICH requirements, for Ozenoxacin and Benzoic acid. Consequently, this method has found to be validated, simple, rapid and successfully applicable, to the simultaneous estimation of Ozenoxacin and Benzoic acid by RP-HPLC, for routine analytical testing in quality control, with a run time of 15 min and for future research studies. Forced degradation of Ozenoxacin cream 1% w/w formulation was performed and found that validated method has stability indicating potential that needs to be further studied.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45513360","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}
Minle Chen, Jia Xu, Feifei Chen, Quan Zhou, Shuanghu Wang, Aixia Han
Ivosidenib (AG-120) is an unlisted, but estimated to be valid, oral inhibitor for isocitrate dehydrogenase 1 (IDH1) in the phase Ⅰ study of IDH1-mutated acute myeloid leukemia (AML) patients. This paper presents the investigation and validation of a rapid, effective, qualitative and quantitative determination method of ivosidenib in rat plasma by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The samples were treated using acetonitrile precipitation to remove protein influence. Then, the supernatant was extracted to analyze plasma concentration traits. In the UPLC system, acetonitrile and water containing 0.1% formic acid were selected as a cosolvent mobile phase, applying a gradient elution to isolate compounds in a C18 column. Mass detections were performed on a triple quadruple mass spectrometer in positive ion mode. Electroshock characteristic fragment ionization was used for m/z 583.95→214.53 for ivosidenib for quantitative determination, m/z 583.95→186.6 for qualitative determination, and m/z 492.06→354.55 for IS. The selectivity, linearity, stability, accuracy and precision were verified by reaching the guideline criteria from European Medicine Agency (EMA) and the Food and Drug Administration (FDA). The calibration curve was linear over the concentration range of 2–2,000 ng mL−1 for ivosidenib in rat plasma with a lower limit of quantification (LLOQ) of at least 2 ng mL−1. Additionally, there was no distinct matrix effect or carry-over phenomenon. The method was successfully established and applied to separate ivosidenib from plasma, with the entire analytical process being performed within 3 min for each sample, which shows high-efficiency and convenience for further studies of ivosidenib.
Ivosidenib (AG-120)是一种未上市但估计有效的口服异柠檬酸脱氢酶1 (IDH1)抑制剂，用于IDH1突变的急性髓性白血病(AML)患者的Ⅰ期研究。建立了一种快速、有效、定性、定量测定大鼠血浆中伊沃西地尼的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。样品用乙腈沉淀法去除蛋白质的影响。然后提取上清液分析血浆浓度特征。在UPLC系统中，选择含有0.1%甲酸的乙腈和水作为共溶剂流动相，在C18柱中采用梯度洗脱分离化合物。在正离子模式下，用三联四联质谱仪进行质量检测。用m/z 583.95→214.53进行ivosidenib定量测定，m/z 583.95→186.6进行定性测定，m/z 492.06→354.55进行IS定量测定。通过符合欧洲药品管理局(EMA)和美国食品药品监督管理局(FDA)的指导标准，验证了该方法的选择性、线性度、稳定性、准确度和精密度。ivosidenib在大鼠血浆浓度2 ~ 2000 ng mL−1范围内呈线性，定量下限(LLOQ)至少为2 ng mL−1。此外，没有明显的基质效应和结转现象。该方法成功建立并应用于ivosidenib与血浆的分离，每个样品的整个分析过程在3 min内完成，为进一步研究ivosidenib提供了高效率和便捷性。
{"title":"Validated UPLC-MS/MS method for the determination of ivosidenib in rat plasma: Application to a pharmacokinetic study","authors":"Minle Chen, Jia Xu, Feifei Chen, Quan Zhou, Shuanghu Wang, Aixia Han","doi":"10.1556/1326.2022.01053","DOIUrl":"https://doi.org/10.1556/1326.2022.01053","url":null,"abstract":"\u0000 Ivosidenib (AG-120) is an unlisted, but estimated to be valid, oral inhibitor for isocitrate dehydrogenase 1 (IDH1) in the phase Ⅰ study of IDH1-mutated acute myeloid leukemia (AML) patients. This paper presents the investigation and validation of a rapid, effective, qualitative and quantitative determination method of ivosidenib in rat plasma by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The samples were treated using acetonitrile precipitation to remove protein influence. Then, the supernatant was extracted to analyze plasma concentration traits. In the UPLC system, acetonitrile and water containing 0.1% formic acid were selected as a cosolvent mobile phase, applying a gradient elution to isolate compounds in a C18 column. Mass detections were performed on a triple quadruple mass spectrometer in positive ion mode. Electroshock characteristic fragment ionization was used for m/z 583.95→214.53 for ivosidenib for quantitative determination, m/z 583.95→186.6 for qualitative determination, and m/z 492.06→354.55 for IS. The selectivity, linearity, stability, accuracy and precision were verified by reaching the guideline criteria from European Medicine Agency (EMA) and the Food and Drug Administration (FDA). The calibration curve was linear over the concentration range of 2–2,000 ng mL−1 for ivosidenib in rat plasma with a lower limit of quantification (LLOQ) of at least 2 ng mL−1. Additionally, there was no distinct matrix effect or carry-over phenomenon. The method was successfully established and applied to separate ivosidenib from plasma, with the entire analytical process being performed within 3 min for each sample, which shows high-efficiency and convenience for further studies of ivosidenib.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-08-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47142753","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}
H. Elmansi, M. El-Awady, S. Barghash, S. A. El-Razeq, F. Belal
A fast reliable micellar electrokinetic methodology was investigated for the concurrent quantitation of six antimicrobial and anti-inflammatory drugs, namely, ciprofloxacin, dexamethasone, metronidazole, ornidazole, spiramycin and tinidazole. The method has the merits of rapidity, precision, and sensitivity. The separation was carried out in less than 7 min by applying a basic background electrolyte consisting of 25 mM disodium tetraborate buffer, pH 9 containing 50 mM SDS at 25 kV using photodiode array detector at 230 and 315 nm. The internal standard used during analysis was cromolyn sodium and validation was carried out following ICH guidelines. The proposed method showed linear response over the range from 0.5 to 10.0 μg mL−1 reaching limits of detection and limits of quantitation in the ranges of 0.09–0.2 μg mL−1 and 0. 27–0.6 respectively. The method's greenness was estimated using the GAPI tool where excellent greenness was concluded. Co-formulated or single-ingredient commercial preparations were investigated and the results were statistically evaluated.
{"title":"Green versatile micellar electrokinetic chromatographic method for determination of six antimicrobial and anti-inflammatory drugs in combined dosage forms","authors":"H. Elmansi, M. El-Awady, S. Barghash, S. A. El-Razeq, F. Belal","doi":"10.1556/1326.2022.01057","DOIUrl":"https://doi.org/10.1556/1326.2022.01057","url":null,"abstract":"\u0000 A fast reliable micellar electrokinetic methodology was investigated for the concurrent quantitation of six antimicrobial and anti-inflammatory drugs, namely, ciprofloxacin, dexamethasone, metronidazole, ornidazole, spiramycin and tinidazole. The method has the merits of rapidity, precision, and sensitivity. The separation was carried out in less than 7 min by applying a basic background electrolyte consisting of 25 mM disodium tetraborate buffer, pH 9 containing 50 mM SDS at 25 kV using photodiode array detector at 230 and 315 nm. The internal standard used during analysis was cromolyn sodium and validation was carried out following ICH guidelines. The proposed method showed linear response over the range from 0.5 to 10.0 μg mL−1 reaching limits of detection and limits of quantitation in the ranges of 0.09–0.2 μg mL−1 and 0. 27–0.6 respectively. The method's greenness was estimated using the GAPI tool where excellent greenness was concluded. Co-formulated or single-ingredient commercial preparations were investigated and the results were statistically evaluated.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-08-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43873965","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}
A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.
建立了一种简便、快速、灵敏的UPLC-MS/MS法测定小鼠血液中的螺旋艾酰胺，并应用于小鼠静脉注射（5 mg kg−1）和口服（20 mg kg−1）给药。在HSS T3柱上，设置为40 °C，用乙腈和0.1%甲酸的流动相梯度洗脱进行色谱分离。在电喷雾（ESI）阳性界面中，采用多重反应监测（MRM）模式对Spiraeoside和内标物（IS）进行定量分析。MRM模式是监测m/z 465.4的碎片→303.1和m/z 451.3→ 螺糖苷和IS分别为289.2。结果表明，在1–200的浓度范围内具有良好的线性关系 ng mL−1（r>0.998），定量下限（LLOQ）为1.0 ng mL−1。该方法的日内和日间精密度（RSD%）在14.0%以内，准确度在90.0%-115.0%之间。雪碧苷的提取回收率优于63.0%，基质效应在86%-98%之间。它还表明半衰期短，小鼠的绝对生物利用度为4.0%。因此，所建立的UPLC-MS/MS方法适用于螺雷酰胺在小鼠体内的药代动力学和生物利用度研究。
{"title":"An UPLC-MS/MS method for quantification of spiraeoside in mouse blood and its application to a pharmacokinetic and bioavailability study","authors":"Xiaojun Cai, Xiangyi Dai, Zhoupeng Li, Junying Chen, Xianqin Wang, Meiling Zhang","doi":"10.1556/1326.2022.01061","DOIUrl":"https://doi.org/10.1556/1326.2022.01061","url":null,"abstract":"\u0000 A simple, rapid, and sensitive method based on UPLC-MS/MS was developed to determine spiraeoside in mouse blood, and was applied to the pharmacokinetics and bioavailability of spiraeoside after mice after intravenous (a dose of 5 mg kg−1) and oral (a dose of 20 mg kg−1) administration. On HSS T3 column set at 40 °C, chromatographic separation was obtained with the mobile phase of acetonitrile and 0.1% formic acid using the gradient elution. Spiraeoside and internal standard (IS) were quantitatively analyzed using multiple reaction monitoring (MRM) mode in electrospray (ESI) positive interface. The MRM mode was monitoring the fragmentation of m/z 465.4→303.1 and m/z 451.3→ 289.2 for spironoside and IS, respectively. The results showed a good linear relationship was in the concentration range of 1–200 ng mL−1 (r > 0.998) and the lower limit of quantification (LLOQ) was 1.0 ng mL−1. The intra- and the inter-day precision (RSD%) of the method was within 14.0%, and the accuracy ranged from 90.0% to 115.0%. The extraction recovery of spriaeoside was better than 63.0%, and the matrix effects were in the range of 86%–98%. It also showed the half-life was short, and the absolute bioavailability was 4.0% in mice. Therefore, the established UPLC-MS/MS method was suitable for the pharmacokinetic and bioavailability study of spiraeoside in mice.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-08-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41935238","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}
In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with both detection techniques such as diode-array detection and fluorescence detection (HPLC-DAD-FLD) for the determination of nesfatin-1 in fetal bovine serum samples. The limit of detection (LOD) and limit of quantification (LOQ) for nesfatin-1 were set at satisfactory values in the range 0.22–0.35 mg mL−1 and in the range 0.67–1.05 mg mL−1, respectively (at two different wavelengths (DAD) and at four different wavelengths (FLD)). Analyte concentrations were determined as the average value from fetal bovine serum matrix samples. The preliminary results show that the SPE procedure on Isolute Si-TsOH (SCX-3) could be used for further nesfatin-1 analyses in human serum samples. Both the SPE technique, chromatographic analysis with gradient elution mode and detection technique are fast and convenient.
在这项研究中，我们提出了一种简单、经济、灵敏的高效液相色谱检测技术，如二极管阵列检测和荧光检测(HPLC-DAD-FLD)，用于测定胎牛血清样品中的nesfatin-1。nesfatin-1的检出限(LOD)和定量限(LOQ)分别在0.22 ~ 0.35 mg mL -1和0.67 ~ 1.05 mg mL -1范围内(两种不同波长(DAD)和四种不同波长(FLD))设定在令人满意的值。分析物浓度测定为胎牛血清基质样品的平均值。初步结果表明，固相萃取法可用于进一步分析人血清样品中的脂质-1。固相萃取技术、梯度洗脱色谱分析和检测技术均具有快速方便的特点。
{"title":"Application of solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) and comparison of both detection techniques (DAD and FLD) to analyse nesfatin-1 in fetal bovine serum samples","authors":"T. Tuzimski, Michał Szubartowski","doi":"10.1556/1326.2022.01076","DOIUrl":"https://doi.org/10.1556/1326.2022.01076","url":null,"abstract":"\u0000 In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with both detection techniques such as diode-array detection and fluorescence detection (HPLC-DAD-FLD) for the determination of nesfatin-1 in fetal bovine serum samples. The limit of detection (LOD) and limit of quantification (LOQ) for nesfatin-1 were set at satisfactory values in the range 0.22–0.35 mg mL−1 and in the range 0.67–1.05 mg mL−1, respectively (at two different wavelengths (DAD) and at four different wavelengths (FLD)). Analyte concentrations were determined as the average value from fetal bovine serum matrix samples. The preliminary results show that the SPE procedure on Isolute Si-TsOH (SCX-3) could be used for further nesfatin-1 analyses in human serum samples. Both the SPE technique, chromatographic analysis with gradient elution mode and detection technique are fast and convenient.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-08-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43768457","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}
A new method for the analysis of four target flavonoids in two kinds of citrus samples by ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed. Main variables affecting the UHPSFC separation were optimized, and under the optimized conditions the four target compounds (tangeretin, nobiletin, hesperetin and naringenin) can be separated within 10 min. The UHPSFC method allowed the determination of the four target compounds in the diluted stock solutions with limit of detection (LOD) ranging from 1.08 to 2.28 μg mL−1, and limit of quantification (LOQ) ranging from 1.45 to 4.52 μg mL−1, respectively. The coefficients of determination (R 2) of the calibration curves were higher than 0.9950. The recoveries of the four target compounds at three different concentrations were in the range of 82.4–117.6%. The validation results demonstrated that the proposed method is simple, accurate, time-saving and environment friendly, and it is applicable to a variety of complex samples such as medicine-food dual purpose herbs and functional foods.
{"title":"Development and validation of ultra-high performance supercritical fluid chromatography method for quantitative determination of four target flavonoids components in citrus samples","authors":"B. Li, Z. Li, Xin Kang Li, Lin Fan Tan","doi":"10.1556/1326.2022.01010","DOIUrl":"https://doi.org/10.1556/1326.2022.01010","url":null,"abstract":"\u0000 A new method for the analysis of four target flavonoids in two kinds of citrus samples by ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed. Main variables affecting the UHPSFC separation were optimized, and under the optimized conditions the four target compounds (tangeretin, nobiletin, hesperetin and naringenin) can be separated within 10 min. The UHPSFC method allowed the determination of the four target compounds in the diluted stock solutions with limit of detection (LOD) ranging from 1.08 to 2.28 μg mL−1, and limit of quantification (LOQ) ranging from 1.45 to 4.52 μg mL−1, respectively. The coefficients of determination (R\u0000 2) of the calibration curves were higher than 0.9950. The recoveries of the four target compounds at three different concentrations were in the range of 82.4–117.6%. The validation results demonstrated that the proposed method is simple, accurate, time-saving and environment friendly, and it is applicable to a variety of complex samples such as medicine-food dual purpose herbs and functional foods.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42570239","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}
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