İbrahim Demir, İbrahim Bulduk, Hüseyin Enginar, Cemal Çifci
Abstract Mirtazapine is an antidepressant medication used to treat the major depressive disorder in adults. In this study, two different chromatographic methods were developed for the determination of mirtazapine in pharmaceutical products. In the first method, An Extend C 18 column (250 × 4.6 mm, 5 μm) was used and the temperature was kept constant at 25 °C. The mobile phase was determined as 0.1% formic acid solution and acetonitrile (80/20, v/v), and isocratic elution was applied. The flow rate of the mobile phase was determined as 1.0 mL min −1 and the injection volume was 20 µL. Detection was performed at 291 nm. using a UV detector. In the second method, ethanol was used as the organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated by ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 µg mL −1 . of mirtazapine. Later, these chromatographic methods were applied to pharmaceutical formulations. Comparison of the obtained results in terms of means was made using Student's ( t ) test, and comparisons in terms of standard deviations were made using the Fischer (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using the AGREE-Analytical GREEnness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of mirtazapine in pharmaceutical formulations.
米氮平是一种用于治疗成人重度抑郁症的抗抑郁药物。建立了两种不同的色谱法测定药品中米氮平的含量。第一种方法采用An Extend C 18色谱柱(250 × 4.6 mm, 5 μm)，温度恒定在25℃。流动相为0.1%甲酸溶液-乙腈(80/20,v/v)，等密度洗脱。流动相流速为1.0 mL min - 1，进样量为20µL。在291 nm处检测。使用紫外线探测器。第二种方法以乙醇为有机改性剂。这些方法之间的唯一区别是有机改性剂。所有方法的其他条件相同。两种色谱方法均通过ICH指南验证了各种参数，如选择性、线性、准确度、精密度、检测和定量限以及鲁棒性。在5 ~ 30µg mL−1的浓度范围内，色谱法的测定系数均大于0.999。米氮平。后来，这些色谱方法被应用于药物制剂。采用Student’s (t)检验比较所得结果的均值，采用Fischer (F)检验比较标准差。结果表明，两种方法间无显著性差异。然后使用AGREE-Analytical GREEnness度量软件对这两种方法进行评估。以乙醇为有机改性剂的色谱法是测定药物制剂中米氮平的一种环境友好的方法。
{"title":"A green HPLC method for determination of mirtazapine in pharmaceutical products: Development, validation, and greenness assessment","authors":"İbrahim Demir, İbrahim Bulduk, Hüseyin Enginar, Cemal Çifci","doi":"10.1556/1326.2023.01155","DOIUrl":"https://doi.org/10.1556/1326.2023.01155","url":null,"abstract":"Abstract Mirtazapine is an antidepressant medication used to treat the major depressive disorder in adults. In this study, two different chromatographic methods were developed for the determination of mirtazapine in pharmaceutical products. In the first method, An Extend C 18 column (250 × 4.6 mm, 5 μm) was used and the temperature was kept constant at 25 °C. The mobile phase was determined as 0.1% formic acid solution and acetonitrile (80/20, v/v), and isocratic elution was applied. The flow rate of the mobile phase was determined as 1.0 mL min −1 and the injection volume was 20 µL. Detection was performed at 291 nm. using a UV detector. In the second method, ethanol was used as the organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated by ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 µg mL −1 . of mirtazapine. Later, these chromatographic methods were applied to pharmaceutical formulations. Comparison of the obtained results in terms of means was made using Student's ( t ) test, and comparisons in terms of standard deviations were made using the Fischer (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using the AGREE-Analytical GREEnness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of mirtazapine in pharmaceutical formulations.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"31 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134975303","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}
Abstract It still remains a great challenge to selectively enrich and sensitively quantify the trace volatile organic compounds (VOCs) in real samples with complex matrix. In this study, an integration method combining a selective enrichment medium of reduced graphene oxide (rGO) with a specially designed micro thermal-assisted purge-and-trap sampling device was developed for efficient enrichment and sensitive quantification of trace tobacco VOCs coupling with thermal desorption (TD)-gas chromatography/mass spectrometry (GC/MS). The prepared rGO has been proved to possess excellent enrichment selectivity and capacity for tobacco polar VOCs with the multi-layer structure, good thermal stability and large specific surface area. The specially designed sampling device was efficient and suitable for enriching and sampling trace polar tobacco VOCs coupling with rGO medium. Under the optimized sampling and analytical conditions, the established analytical method could be actually applied for quantification of typical tobacco polar VOCs with the good recoveries of 72.9–128% and the satisfied RSDs of 1.8–19.9% ( n = 3). The results suggested that the developed method was selective, sensitive and reliable for enrichment and quantification of trace tobacco polar VOCs.
{"title":"Efficient and sensitive quantification of polar tobacco volatile organic compounds by a micro thermal-assisted sampling device using reduced graphene oxide coupling with thermal desorption-gas chromatography/mass spectrometry","authors":"Yanhua Lai, Bing Han, Jiahui Wu, Shouhui Weng, Senlin Chen, Junxia Wang, Yu Wang, Xiaowei Pan, Yun Lin, Hong Tao, Zhuomin Zhang, Gongke Li","doi":"10.1556/1326.2023.01161","DOIUrl":"https://doi.org/10.1556/1326.2023.01161","url":null,"abstract":"Abstract It still remains a great challenge to selectively enrich and sensitively quantify the trace volatile organic compounds (VOCs) in real samples with complex matrix. In this study, an integration method combining a selective enrichment medium of reduced graphene oxide (rGO) with a specially designed micro thermal-assisted purge-and-trap sampling device was developed for efficient enrichment and sensitive quantification of trace tobacco VOCs coupling with thermal desorption (TD)-gas chromatography/mass spectrometry (GC/MS). The prepared rGO has been proved to possess excellent enrichment selectivity and capacity for tobacco polar VOCs with the multi-layer structure, good thermal stability and large specific surface area. The specially designed sampling device was efficient and suitable for enriching and sampling trace polar tobacco VOCs coupling with rGO medium. Under the optimized sampling and analytical conditions, the established analytical method could be actually applied for quantification of typical tobacco polar VOCs with the good recoveries of 72.9–128% and the satisfied RSDs of 1.8–19.9% ( n = 3). The results suggested that the developed method was selective, sensitive and reliable for enrichment and quantification of trace tobacco polar VOCs.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"20 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135592263","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}
Kai Li, Liqiang Guo, Guoning Tian, Xiaojie Xu, Yajing Li
Abstract A highly accurate and precise method for the simultaneous detection of 18 neonicotinoids and their metabolites in meat was developed using liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). To improve the pretreatment step of the method, five different commercially available clean-up materials (including C18+PSA (primary secondary amine), Z-Sep (with Discover DSC-C18), EMR-Lipid, SHIMSEN QuEChERS, and Clean-up LPAS) were studied in the treatment of three meat matrices: pork, duck and yellow croaker. Based on the recovery data, we found that among the five purification materials, SHIMSEN QuEChERS was slightly more effective than the others for 18 neonicotinoids. Therefore, SHIMSEN QuEChERS was used as the purification sorbent, and the extraction solvents, extraction methods and chromatographic and mass spectrometric conditions were optimized. A matrix-matched calibration method was applied for quantification. In three different meat matrixes (pork, duck, and yellow croaker), all the target compounds showed good linearity, both with values of r 2 > 0.995. The average recovery of all neonicotinoids ranges from 63.4 to 114.2% (pork), 63.0–113.2% (duck), and 63.9–110.5% (yellow croaker). Relative standard deviations were all <15% for intraday and interday precision. The values of limit of detection (LOD) and limit of quantification (LOQ) were, respectively, ranging from 0.04 to 1.0 μg kg −1 and 0.10 to 2.0 μg kg −1 . Compared with previous reports, this method has advantage in LOQs, indicating that it it may be a preferred choice for the detection of neonicotinoid pesticides in meat samples.
{"title":"Evaluation of various commercial lipid removal sorbents for the detection of 18 neonicotinoid insecticides and their metabolites in meat by liquid chromatography tandem mass spectrometry","authors":"Kai Li, Liqiang Guo, Guoning Tian, Xiaojie Xu, Yajing Li","doi":"10.1556/1326.2023.01170","DOIUrl":"https://doi.org/10.1556/1326.2023.01170","url":null,"abstract":"Abstract A highly accurate and precise method for the simultaneous detection of 18 neonicotinoids and their metabolites in meat was developed using liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). To improve the pretreatment step of the method, five different commercially available clean-up materials (including C18+PSA (primary secondary amine), Z-Sep (with Discover DSC-C18), EMR-Lipid, SHIMSEN QuEChERS, and Clean-up LPAS) were studied in the treatment of three meat matrices: pork, duck and yellow croaker. Based on the recovery data, we found that among the five purification materials, SHIMSEN QuEChERS was slightly more effective than the others for 18 neonicotinoids. Therefore, SHIMSEN QuEChERS was used as the purification sorbent, and the extraction solvents, extraction methods and chromatographic and mass spectrometric conditions were optimized. A matrix-matched calibration method was applied for quantification. In three different meat matrixes (pork, duck, and yellow croaker), all the target compounds showed good linearity, both with values of r 2 > 0.995. The average recovery of all neonicotinoids ranges from 63.4 to 114.2% (pork), 63.0–113.2% (duck), and 63.9–110.5% (yellow croaker). Relative standard deviations were all <15% for intraday and interday precision. The values of limit of detection (LOD) and limit of quantification (LOQ) were, respectively, ranging from 0.04 to 1.0 μg kg −1 and 0.10 to 2.0 μg kg −1 . Compared with previous reports, this method has advantage in LOQs, indicating that it it may be a preferred choice for the detection of neonicotinoid pesticides in meat samples.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"87 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-10-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135739029","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}
Zhengming Qian, J. Chen, Qing-Qing Lei, Da Li, Guoying Tan, Juying Xie, Wenqing Li
An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.
采用液相色谱-质谱联用技术建立了穿心莲中穿心莲内酯和脱水穿心莲苷的超快速分析方法。用10 mL 40%（v/v）甲醇，然后用C18固相萃取柱纯化。LC分离在Poroshell 120上进行 EC-C18柱（30 × 2.1 毫米，2.7 μm），用0.5洗脱 mmol L−1乙酸铵水溶液和乙腈（65:35），流速为0.7 mL min−1，并通过质谱法（MS）进行检测。LC-MS分析时间小于1 min.新方法具有良好的线性（r＞0.9900）、精密度和重复性（RSD<2.0%），穿心莲内酯和脱氢穿心莲苷的回收率分别为93.5%（RSD=2.2%）和97.7%（RSD=2.4%）。该方法已成功应用于7批AH样品中穿心莲内酯和脱水穿心莲固体的测定，所有样品中分析物的含量均符合中国药典的相关验收标准（>0.8%），这将有助于提高AH样本测试的效率和降低成本。
{"title":"Ultra-rapid determination of andrographolide and dehydroandrographolide in Andrographis Herba by solid phase extraction and liquid chromatography with mass spectrometry","authors":"Zhengming Qian, J. Chen, Qing-Qing Lei, Da Li, Guoying Tan, Juying Xie, Wenqing Li","doi":"10.1556/1326.2023.01156","DOIUrl":"https://doi.org/10.1556/1326.2023.01156","url":null,"abstract":"An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49366115","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. Fouad, Ahmed S Abdelkhalek, Hisham Elrefay, Hany A. Batakoushy, M. K. Soltan
A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank.
{"title":"The use of an RP-HPLC-UV method for the analysis of oxcarbazepine in the presence of its preservatives; stability studies and application to human plasma samples","authors":"A. Fouad, Ahmed S Abdelkhalek, Hisham Elrefay, Hany A. Batakoushy, M. K. Soltan","doi":"10.1556/1326.2023.01157","DOIUrl":"https://doi.org/10.1556/1326.2023.01157","url":null,"abstract":"A simple, sensitive, selective, accurate and precise method was developed and fully validated for determination of oxcarbazepine (OXC) in presence of their preservatives and determination of oxcarbazepine (OXC) in human plasma. A reversed phase liquid chromatography (RP-HPLC) with UV detection techniques were applied for separation and quantification of studied drug OXC. Successful separation of the drug from methyl paraben (M.P.), propyl paraben (P.P.) and potassium sorbate (P.ST.) was achieved on a Kromasil C18 column (5 μm particle size, pore size 300 Å, l × I.D. 250 × 4.6 mm). The mobile phase that contain aqueous 0.05M potassium dihydrogen phosphate buffer (pH 7): acetonitrile, (50: 50, %v/v). The method was linear over concentration ranges 5.0–50 μg mL−1 for OXC. Bioanalytical validation of the developed method was carried out according to US-FDA guidelines and revealed a good linear relations over a range of (5.0–50), (0.5–10), (0.05–0.15), and (1.0–10) μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, with a correlation coefficient (R2) of more than 0.999. Limit of detection (LOD) were 1.15, 0.03, 0.01 and 0.04 μg mL−1 for OXC, M.P, P.P, and P.ST, respectively, Intra and inter-day precisions, calculated as percentage relative standard deviation (% RSD), were lower than 2.0%. The developed method can be applied for routine drug analysis, therapeutic drug monitoring and bioequivalence studies through the analysis of plasma samples taken from blood bank.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46859556","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}
Nabil N. Al-Hashimi, Rand O. Shahin, A. El-Sheikh, Malak Jibreel, Nada Alsakhen, A. Alqudah, Muna Oqal, Jafar I. Abdelghani
The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument.
尿8-羟基-2′-脱氧鸟苷(8-OHdG)是多种疾病特别是癌症的氧化应激生物标志物，其浓度水平被认为是一种适合诊断的途径。尿8-OHdG的测定是具有挑战性的，因为它在一个复杂的基质中的低水平。在本研究中，建立了一种高效液相色谱二极管阵列检测(HPLC-DAD)分析前的固/液相微萃取技术，用于测定尿样中痕量8-OHdG。该固/液相微萃取装置是将多壁碳纳米管补强于两端热封的2.5 cm短段中空纤维微管的孔内。根据优化后的程序，将选定的分析物从酸性样品溶液(pH = 5调整为10ml)中提取到五个提取装置中。提取时间(30 min)结束后，用甲醇(350µL)在超声下洗脱5 min。该方法在合成尿液样品中具有良好的线性关系(R2 = 0.999)，检出限为0.85 ng mL−1，提取回收率为92.36%。与其他已发表的方法相比，所建立的微萃取技术具有可靠的灵敏度、可行的操作方法和简单的操作方法，可用于使用廉价且常用的HPLC-DAD仪器测定尿癌患者样品中的痕量8-OHdG。
{"title":"A new approach for determination of urinary 8-hydroxy-2′-deoxyguanosine in cancer patients using reinforced solid/liquid phase microextraction combined with HPLC-DAD","authors":"Nabil N. Al-Hashimi, Rand O. Shahin, A. El-Sheikh, Malak Jibreel, Nada Alsakhen, A. Alqudah, Muna Oqal, Jafar I. Abdelghani","doi":"10.1556/1326.2023.01142","DOIUrl":"https://doi.org/10.1556/1326.2023.01142","url":null,"abstract":"The concentration level of urinary 8-hydroxy-2′-deoxyguanosine (8-OHdG), an oxidative stress biomarker for various diseases especially cancer, has been attracted as a pathway suitable for diagnostic purposes. Determination of urinary 8-OHdG is challenging due to its low level within a complex matrix. In this study, a new approach of solid/liquid phase microextraction technique prior to high-performance liquid chromatography diode-array detection (HPLC-DAD) analysis was developed for the determination of trace levels of 8-OHdG in urine samples. The solid/liquid phase microextraction device was constructed by reinforcement of multi-walled carbon nanotubes into the pores of a short segment 2.5 cm of hollow fiber microtube with two ends heat sealed. Based on the optimized procedure, the selected analyte was extracted from an acidic sample solution (10 mL adjusted at pH = 5) into the five extraction devices. After the extraction period (30 min), the 8-OHdG was eluted from the extraction device using methanol (350 µL) under ultrasonication for 5 min. The analytical performance of the method in synthetic urine samples showed good linearity (R2 > 0.999) with the limits of detection of 0.85 ng mL−1, and extraction recovery > 92.36%. The developed microextraction technique exhibited a confident sensitivity, feasible operation, and simplicity in comparison with other published methods and was valid to determinate trace 8-OHdG in urine cancer patients' samples by using a cheap and commonly available HPLC-DAD instrument.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49007615","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}
Osama I. Abdallah, N. S. Ahmed, Rania M. Abd El-Hamid, S. Alhewairini
Residues of the fungicides difenoconazole, propiconazole, cyflufenamid, and mandipropamid were determined in tomato fruit using acetonitrile for extraction and LC-MS/MS for quantification. Validation criteria include linearity range, the limit of detection (LOD) and limit of quantitation (LOQ), accuracy in terms of precision and trueness, and matrix effect were studied. The recovery rates of the method ranged from 91.8 to 106.3%. The precision of the method in terms of repeatability at one day (RSDr) and between three days (RSDR) ranged from 2.8 to 6.4% and from 4.3 to 7.6%, respectively, with good trueness from 92.2 to 96.4%. Matrix effects (suppression effects) ranged from 3.8% to 11.1%. The validated method was used to evaluate the dissipation kinetics of three different premix formulations: 30% EC (15% difenoconazole + 15% propiconazole), 14% DC (12.5% difenoconazole + 1.5% cyflufenamid), and 50% SC (25% difenoconazole + 25% mandipropamid) used on field tomatoes in Egypt. A first-order kinetic equation best describes residue dissipation. The calculated half-lives of difenoconazole, propiconazole, cyflufenamid, and mandipropamid were 2.01–2.27, 1.89, 1.97, and 1.71 days, respectively. The dissipation rate of difenoconazole did not differ significantly in the three premix formulations. Mandipropamid also dissipated faster compared to the other fungicides tested. The chronic dietary risk assessment results showed a minimal risk to adult Egyptian consumers. Waiting periods were advised for the safe consumption of tomatoes treated with the tested premix formulations.
{"title":"Residues of difenoconazole in various ready premixes with propiconazole, cyflufenamid, and mandipropamid in/on tomato fruits","authors":"Osama I. Abdallah, N. S. Ahmed, Rania M. Abd El-Hamid, S. Alhewairini","doi":"10.1556/1326.2023.01134","DOIUrl":"https://doi.org/10.1556/1326.2023.01134","url":null,"abstract":"Residues of the fungicides difenoconazole, propiconazole, cyflufenamid, and mandipropamid were determined in tomato fruit using acetonitrile for extraction and LC-MS/MS for quantification. Validation criteria include linearity range, the limit of detection (LOD) and limit of quantitation (LOQ), accuracy in terms of precision and trueness, and matrix effect were studied. The recovery rates of the method ranged from 91.8 to 106.3%. The precision of the method in terms of repeatability at one day (RSDr) and between three days (RSDR) ranged from 2.8 to 6.4% and from 4.3 to 7.6%, respectively, with good trueness from 92.2 to 96.4%. Matrix effects (suppression effects) ranged from 3.8% to 11.1%. The validated method was used to evaluate the dissipation kinetics of three different premix formulations: 30% EC (15% difenoconazole + 15% propiconazole), 14% DC (12.5% difenoconazole + 1.5% cyflufenamid), and 50% SC (25% difenoconazole + 25% mandipropamid) used on field tomatoes in Egypt. A first-order kinetic equation best describes residue dissipation. The calculated half-lives of difenoconazole, propiconazole, cyflufenamid, and mandipropamid were 2.01–2.27, 1.89, 1.97, and 1.71 days, respectively. The dissipation rate of difenoconazole did not differ significantly in the three premix formulations. Mandipropamid also dissipated faster compared to the other fungicides tested. The chronic dietary risk assessment results showed a minimal risk to adult Egyptian consumers. Waiting periods were advised for the safe consumption of tomatoes treated with the tested premix formulations.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-06-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45732570","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}
{"title":"In memoriam Professor Dr Teresa Kowalska (1946–2023)","authors":"","doi":"10.1556/1326.2023.11111","DOIUrl":"https://doi.org/10.1556/1326.2023.11111","url":null,"abstract":"","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-05-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42548136","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 novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect.
研制了一种新型盐酸阿霉素脂质体注射液，以降低其毒副作用，延长其血浆半衰期。本研究建立并验证了一种快速灵敏的生物分析方法，以表征静脉输注阿霉素注射液后3例中国患者血浆中总阿霉素和游离阿霉素的药动学特征。血浆样品采用蛋白沉淀法测定总阿霉素，固相萃取法测定游离阿霉素。血浆样品预处理后，使用经过验证的LC-MS/MS方法分别定量总浓度和游离浓度。总阿霉素在0.20 ~ 500.0 ng mL−1范围内与游离阿霉素在1.00 ~ 1000 ng mL−1范围内呈线性关系。血浆中游离浓度仅为总水平的六分之一至四分之一。阿霉素脂质体的表观半衰期(50 h)比文献中报道的非靶向药物(<10 h)更长。分布的体积更小。该新型注射制剂可长期稳定地从脂质体中释放游离阿霉素，减少心脏毒副作用，同时保证临床疗效。
{"title":"Development and validation of an LC-MS/MS method for the quantification of free and total doxorubicin in human plasma and its clinical application for a novel doxorubicin hydrochloride liposome injection in Chinese patients with breast cancer","authors":"Keyu Zhang, Daqing Zhang, Z. Ge, F. Qiu","doi":"10.1556/1326.2023.01129","DOIUrl":"https://doi.org/10.1556/1326.2023.01129","url":null,"abstract":"A novel doxorubicin hydrochloride liposome injection was prepared to reduce toxicity and side effects, as well as extend plasma half-life in the treatment of breast cancer. In this study, a rapid and sensitive bioanalytical method was developed and validated to characterize the pharmacokinetic profile of total and free doxorubicin in plasma of 3 Chinese patients after intravenous infusion of this injection. Plasma samples were prepared by protein precipitation for the determination of total doxorubicin, while solid phase extraction was used to determine free doxorubicin. After plasma sample pre-treatment, total and free concentrations were quantified individually using a validated LC-MS/MS method. The calibration curves were found to be linear in the range of 0.20–500.0 ng mL−1 for total doxorubicin and in the range of 1.00–1,000 ng mL−1 for free doxorubicin. The free concentrations in plasma were only one sixth to one quarter of the total levels. Liposomal doxorubicin had a longer apparent half-life (>50 h) than the non-targeted drug (<10 h) reported in the reference. and a lower volume of distribution. This novel injectable formulation steadily released free doxorubicin from liposomes over a long period of time to reduce cardiac toxicity and side effects, while ensuring a clinical curative effect.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-05-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42950221","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}
Almaz Arage, Thomas Layloff, Ariaya Hymete, Ayenew Ashenef
"Corrigendum to: High performance thin layer chromatography (HPTLC) method development and validation for the simultaneous determination of paracetamol, caffeine, chlorpheniramine and phenylepherine in tablet formulation" published on 11 Aug 2022 by Akadémiai Kiadó.
{"title":"Corrigendum to: High performance thin layer chromatography (HPTLC) method development and validation for the simultaneous determination of paracetamol, caffeine, chlorpheniramine and phenylepherine in tablet formulation","authors":"Almaz Arage, Thomas Layloff, Ariaya Hymete, Ayenew Ashenef","doi":"10.1556/1326.2022.11028","DOIUrl":"https://doi.org/10.1556/1326.2022.11028","url":null,"abstract":"\"Corrigendum to: High performance thin layer chromatography (HPTLC) method development and validation for the simultaneous determination of paracetamol, caffeine, chlorpheniramine and phenylepherine in tablet formulation\" published on 11 Aug 2022 by Akadémiai Kiadó.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"5 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-04-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135066137","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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