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A Photo Stability Indicating HPLC technique for Validation of Netupitant and Palonosetron in Bulk and Formulations 奈吡坦和帕洛诺司琼原料药和制剂的光稳定性指示高效液相色谱验证技术
Pub Date : 2020-08-31 DOI: 10.33974/ijrpca.v1i4.220
P. Salomi, B. Sireesha, Afreen Sultana, R. Reddy
Analytical chemistry is the science that seeks ever improved means of measuring the chemical composition of natural and artificial materials.Netupitant Delayed emesis has been largely associated with the activation of tachykinin family neurokinin 1 receptors. Palonosetron is a selective serotonin 5-HT3 receptor antagonist. The antiemetic activity of the drug is brought about through the inhibition of 5-HT3 receptors present both centrally  and peripherally in turn inhibits the visceral afferent stimulation of the vomiting center.The mobile phase used was orthophosphoric and acetate 70% buffer pH 3 and 30% methanol.The assay of Netupitant and Palanosetron was performed with tablets and the % assay was found to be 100.08 and 100.04, The linearity was found to be linear with a correlation coefficient of 0.999, the precision 0.8 and 0.3 for Netupitant and Palanosetron which shows that the method is precise.The validation of developed method shows that the accuracy is well within the limit, which shows that the method is capable of showing good accuracy and reproducibility. The LOD and LOQ for Netupitant were found to be 3.02 and 9.98 and LOD and LOQ for Palanosetron was found to be 3.00 and 10.00. Thus, it shows that the method is stability indicating, sensitive, accurate, robust and precise. Hence, the developed HPLC method can be successfully applied to the pharmaceutical dosage form and can be used for routine analysis.      
分析化学是一门寻求不断改进测量天然和人造材料化学成分的方法的科学。Netupitant延迟呕吐在很大程度上与速激肽家族神经激肽1受体的激活有关。帕洛诺司琼是一种选择性5-羟色胺5-HT3受体拮抗剂。该药物的止吐活性是通过抑制中枢和外周存在的5-HT3受体来实现的,从而抑制呕吐中枢的内脏传入刺激。流动相为正磷酸盐和乙酸酯,pH = 70%缓冲液,甲醇= 30%。采用片剂对尼图匹坦和帕拉诺司琼的含量进行测定,其%含量分别为100.08和100.04,线性关系良好,相关系数分别为0.999,精密度分别为0.8和0.3,表明方法精密度高。方法的验证结果表明,该方法的准确度完全在限定范围内,具有良好的准确度和重复性。Netupitant的LOD和LOQ分别为3.02和9.98,Palanosetron的LOD和LOQ分别为3.00和10.00。结果表明,该方法指示稳定、灵敏、准确、鲁棒性强、精度高。因此,所建立的高效液相色谱法可以成功地应用于药物剂型的分析,并可用于常规分析。
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引用次数: 1
Method developed for the determination of apixaban by using U.V. spectrophotometric 建立了紫外分光光度法测定阿哌沙班的方法
Pub Date : 2019-07-29 DOI: 10.33974/ijrpca.v1i3.115
B. Mahendra, K. H. Sundari, T. Vimalakkannan
The present work is aim to Develop UV spectrophotometry method for the estimation of Apixaban in its dosage forms. Analysed the marketed formulations for their reliability and accuracy and Performed the recovery studies for the developed UV spectrophotometric method. The developed method was validate for its accuracy precision reproducibility. On the basis of results the UV spectrophotometric method developed for the determination of Apixaban is found to be precise, accurate and cost effective. Hence this method can be used for routine analysis of Apixaban in bulk and pharmaceutical dosage forms.
本工作旨在建立紫外分光光度法测定阿哌沙班剂型的方法。分析了市售制剂的可靠性和准确性,并对所开发的紫外分光光度法进行了回收率研究。该方法的准确度、精密度、重复性良好。结果表明,紫外分光光度法测定阿哌沙班的准确度高、准确度高、成本效益好。因此,该方法可用于阿哌沙班原料药和药物剂型的常规分析。
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引用次数: 3
A new analytical method for determination of dolutegravir and rilpivirine in pharmaceutical formulations by RP-HPLC method 建立了反相高效液相色谱法测定制剂中多替格拉韦和利匹韦林含量的新方法
Pub Date : 2019-07-28 DOI: 10.33974/ijrpca.v1i3.119
Kanchipogu usha rani, P. V. Rao, N. Rao
A simple, rapid, precise, sensitive and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the quantitative analysis of Dolutegravir and Rilpivirine in pharmaceutical dosage form. Chromatographic separation of Dolutegravir and Rilpivirine was achieved on Waters Alliance -2695, by using Luna C18 (250mm x 4.6mm, 5µm) column and the mobile phase containing 0.1% OPA & ACN in the ratio of 50:50 v/v. The flow rate was 1.0 ml/min, detection was carried out by absorption at 245 nm using a photodiode array detector at ambient temperature. The number of theoretical plates and tailing factor for Dolutegravir and Rilpivirine were NLT 2000 and should not more than 2 respectively. The linearity of the method was excellent over the concentration range 10-150 µg/ml and 5-75 µg/ml for Dolutegravir and Rilpivirine respectively. The correlation coefficient was 0.999. % Relative standard deviation of peak areas of all measurements always less than 2.0. The proposed method was validated according to ICH guidelines. The method was found to be simple, economical, suitable, precise, accurate & robust method for quantitative analysis of Dolutegravir and Rilpivirine study of its stability.
建立了一种简便、快速、精确、灵敏、重现性好的反相高效液相色谱(RP-HPLC)定量分析药物剂型多替格拉韦和利匹韦林的方法。Dolutegravir和Rilpivirine的色谱分离采用Waters Alliance -2695,色谱柱为Luna C18 (250mm × 4.6mm, 5µm),流动相含0.1% OPA和ACN,比例为50:50 v/v。流速为1.0 ml/min,室温下采用光电二极管阵列检测器在245 nm处吸收检测。Dolutegravir和Rilpivirine的理论极板数和尾尾因子分别为nlt2000,不大于2。dolutegravity和Rilpivirine分别在10 ~ 150µg/ml和5 ~ 75µg/ml的浓度范围内线性良好。相关系数为0.999。所有测量峰面积的相对标准偏差总是小于2.0。根据ICH指南对该方法进行了验证。结果表明,该方法简便、经济、适用、精密度高、准确度高、稳健性好,可用于多替格拉韦和利匹韦林的定量分析。
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引用次数: 3
A new analytical method for determination of tenofovir disoproxil fumarate and emtricitabine in pharmaceutical formulations by RP-HPLC method 建立了反相高效液相色谱法测定制剂中富马酸替诺福韦和恩曲他滨含量的新方法
Pub Date : 2019-07-28 DOI: 10.33974/ijrpca.v1i3.118
P. Vani
A simple, rapid, precise, sensitive and reproducible reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the quantitative analysis of Tenofovir Disoproxil Fumarate and Emtricitabine in pharmaceutical dosage form. Chromatographic separation of Tenofovir Disoproxil Fumarate and Emtricitabine was achieved on Waters Alliance -2695, by using Luna C18 (250mm x 4.6mm, 5µm) column and the mobile phase containing 0.1% TEA adjusted pH-2.5 with OPA & ACN in the ratio of 60:40 v/v. The flow rate was 1.0 ml/min, detection was carried out by absorption at 261 nm using a photodiode array detector at ambient temperature. The number of theoretical plates and tailing factor for Tenofovir Disoproxil Fumarate and Emtricitabine were NLT 2000 and should not more than 2 respectively. The linearity of the method was excellent over the concentration range 30-450 µg/ml and 20-300 µg/ml for Tenofovir Disoproxil Fumarate and Emtricitabine respectively. The correlation coefficient was 0.999. % Relative standard deviation of peak areas of all measurements always less than 2.0. The proposed method was validated according to ICH guidelines. The method was found to be simple, economical, suitable, precise, accurate & robust method for quantitative analysis of Tenofovir Disoproxil Fumarate and Emtricitabine study of its stability.
建立了一种简便、快速、精确、灵敏、重现性好的反相高效液相色谱(RP-HPLC)方法,用于富马酸替诺福韦二氧吡酯和恩曲他滨药物剂型的定量分析。采用Waters Alliance -2695,色谱柱为Luna C18 (250mm × 4.6mm, 5µm),流动相为0.1% TEA调整pH-2.5, OPA和ACN的比例为60:40 v/v,对富马酸替诺福韦二氧吡酯和恩曲他滨进行色谱分离。流速为1.0 ml/min,室温下采用光电二极管阵列检测器在261 nm处吸收检测。富马酸替诺福韦和恩曲他滨的理论板数和尾因子分别为nlt2000和不大于2。富马酸替诺福韦二氧吡酯和恩曲他滨在30 ~ 450µg/ml和20 ~ 300µg/ml浓度范围内线性良好。相关系数为0.999。所有测量峰面积的相对标准偏差总是小于2.0。根据ICH指南对该方法进行了验证。该方法简便、经济、适用、精密度高、准确度高、稳扎稳打,可用于富马酸替诺福韦二氧吡酯的定量分析和恩曲他滨的稳定性研究。
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引用次数: 1
A new analytical method for determination of ledipasvir and sofosbuvir in pharmaceutical formulations by HPLC method 建立了高效液相色谱法测定制剂中雷地帕韦和索非布韦含量的新方法
Pub Date : 2019-07-09 DOI: 10.33974/ijrpca.v1i3.113
K. Swathi, P. V. Rao, N. Rao
A simple, Accurate, precise method was developed for the simultaneous estimation of the Sofosbuvir and Ledipasvir in Tablet dosage form. Chromatogram was run through Std Discovery C8 150 x 4.6 mm, 5m. Mobile phase containing Buffer 0.1% OPA: Acetonitrile taken in the ratio 60:40 was pumped through column at a flow rate of 1 ml/min. Buffer used in this method was 0.1% OPA buffer. Temperature was maintained at 30°C. Optimized wavelength selected was 260 nm. Retention time of Sofosbuvir and Ledipasvir were found to be 2.367 min and 3.436 min. %RSD of the Sofosbuvir and Ledipasvir were and found to be 0.6 and 0.5 respectively. %Recovery was obtained as 99.61% and 99.80% for Sofosbuvir and Ledipasvir respectively. LOD, LOQ values obtained from regression equations of Sofosbuvir and Ledipasvir were 0.67, 2.02 and 0.70, 2.12 respectively. Regression equation of Sofosbuvir is y = 4266.x + 7700, and y = 4861.x + 2656.of Ledipasvir. Retention times were decreased and run time was decreased, so the method developed was simple and economical that can be adopted in regular Quality control test in Industries.
建立了同时测定索非布韦和来地帕韦片剂中索非布韦和来地帕韦含量的简便、准确、精确的方法。通过Std Discovery C8 150 x 4.6 mm, 5m进行色谱分析。流动相含0.1% OPA缓冲液:乙腈,比例为60:40,以1ml /min的流速泵入柱中。本方法所用缓冲液为0.1% OPA缓冲液。温度保持在30°C。优选波长为260 nm。索非布韦和来地帕韦的滞留时间分别为2.367 min和3.436 min。索非布韦和来地帕韦的RSD分别为0.6和0.5 %。索非布韦和来地帕韦的回收率分别为99.61%和99.80%。索非布韦和来地帕韦的LOD、LOQ分别为0.67、2.02和0.70、2.12。索非布韦的回归方程为y = 4266。X + 7700和y = 4861。X + 2656。Ledipasvir。该方法减少了滞留时间,缩短了运行时间,简便、经济,可用于工业中常规的质量控制试验。
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引用次数: 1
Stability indicating method development and validation for the determination of haloperidol and benzhexol by RP-HPLC 反相高效液相色谱法测定氟哌啶醇和苯甲醚的稳定性指示方法的建立和验证
Pub Date : 2019-06-08 DOI: 10.33974/ijrpca.v1i2.77
M. Syamala, S. Angalaparameswari, T. Vimalakkannan, C. Sumanjali, T. Jyotshna
A simple, Accurate, precise method was developed for the simultaneous estimation of the Haloperidol and Benzhexol in Tablet dosage form. The chromatogram was run through Kromasil (250mm 4.6mm, 5µ). Mobile phase containing Buffer and Acetonitrile and methanol in the ratio of 48:52 was pumped through column at a flow rate of 1.0 ml/min. The temperature was maintained at 30°C. The optimized wavelength for Haloperidol and Benzhexol was 220nm. The retention time of Haloperidol and Benzhexol were found to be 2.415 min and 2.820min. %RSD of the Haloperidol and Benzhexol were and found to be 0.6 and 0.2 respectively. %Recover was Obtained as 98.92% and 99.60% for Haloperidol and Benzhexol. LOD, LOQ values were obtained from regression equations of Haloperidol and Benzhexol were 0.42ppm, 1.27ppm and 0.04ppm, 0.14ppm respectively. Regression equation of Haloperidol is y = 24009x + 38704, and of Benzhexol is y = 40558x + 2880. Retention times are decreased and that run time was decreased so the method developed was simple and economical that can be adopted in regular Quality control test in Industries
建立了一种简便、准确、精密度高的同时测定片剂中氟哌啶醇和苯甲醚的方法。色谱柱为Kromasil (250mm 4.6mm, 5µ)。以1.0 ml/min的流速将含有缓冲液和乙腈、甲醇的流动相以48:52的比例泵入柱中。温度保持在30℃。氟哌啶醇和苯甲醚的最佳波长为220nm。氟哌啶醇和苯甲醚的滞留时间分别为2.415 min和2.820min。氟哌啶醇和苯甲醚的RSD分别为0.6和0.2。氟哌啶醇和苯甲醚的回收率分别为98.92%和99.60%。氟哌啶醇和苯甲醚的LOD、LOQ分别为0.42ppm、1.27ppm和0.04ppm、0.14ppm。氟哌啶醇的回归方程为y = 24009x + 38704,苯甲醚的回归方程为y = 40558x + 2880。该方法减少了滞留时间,缩短了运行时间,简便、经济,可用于工业中常规的质量控制试验
{"title":"Stability indicating method development and validation for the determination of haloperidol and benzhexol by RP-HPLC","authors":"M. Syamala, S. Angalaparameswari, T. Vimalakkannan, C. Sumanjali, T. Jyotshna","doi":"10.33974/ijrpca.v1i2.77","DOIUrl":"https://doi.org/10.33974/ijrpca.v1i2.77","url":null,"abstract":"A simple, Accurate, precise method was developed for the simultaneous estimation of the Haloperidol and Benzhexol in Tablet dosage form. The chromatogram was run through Kromasil (250mm 4.6mm, 5µ). Mobile phase containing Buffer and Acetonitrile and methanol in the ratio of 48:52 was pumped through column at a flow rate of 1.0 ml/min. The temperature was maintained at 30°C. The optimized wavelength for Haloperidol and Benzhexol was 220nm. The retention time of Haloperidol and Benzhexol were found to be 2.415 min and 2.820min. %RSD of the Haloperidol and Benzhexol were and found to be 0.6 and 0.2 respectively. %Recover was Obtained as 98.92% and 99.60% for Haloperidol and Benzhexol. LOD, LOQ values were obtained from regression equations of Haloperidol and Benzhexol were 0.42ppm, 1.27ppm and 0.04ppm, 0.14ppm respectively. Regression equation of Haloperidol is y = 24009x + 38704, and of Benzhexol is y = 40558x + 2880. Retention times are decreased and that run time was decreased so the method developed was simple and economical that can be adopted in regular Quality control test in Industries","PeriodicalId":14207,"journal":{"name":"International Journal of Research In Pharmaceutical Chemistry and Analysis","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2019-06-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84655866","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 2
Spectrophotometric determination and estimation of minoxidil in tablet dosage form by UV 紫外分光光度法测定片剂中米诺地尔的含量
Pub Date : 2019-05-06 DOI: 10.33974/ijrpca.v1i2.73
S. Khadeerunnisa, T. Vimalakkannan, T. Lakshmi
A simple, precise, accurate and economical UV spectrophotometric method has been developed and validated for the estimation of Minoxidil in the tablet dosage form. Minoxidil shows maximum absorbance at 279.4nm. The method was carried out by using 0.1N HCl as a solvent. The drug shows linearity from the concentration range of 1-6µg/ml and correlation coefficient was found to be 0.9992. The proposed method was statistically validated for precision, accuracy, ruggedness, robustness, the limit of detection, quantitation as per the ICH guidelines. Hence this method can be successfully applied for routine analysis of Minoxidil in bulk and tablet dosage form.
建立了一种简便、精确、准确、经济的米诺地尔片剂紫外分光光度法。米诺地尔在279.4nm处显示最大吸光度。该方法以0.1盐酸为溶剂进行。在1 ~ 6µg/ml浓度范围内呈线性关系,相关系数为0.9992。根据ICH指南对该方法的精密度、准确度、坚固性、稳健性、检出限和定量进行了统计验证。该方法可用于米诺地尔原料药和片剂的常规分析。
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引用次数: 1
Stability indicating RP-HPLC method development and validation for the simultaneous estimation of ceftriaxone and tazobactum in sterile powder for injection 稳定性指示反相高效液相色谱法同时测定注射用无菌散中头孢曲松和他唑巴坦的含量
Pub Date : 2019-04-15 DOI: 10.33974/ijrpca.v1i2.62
T. Vimalakkannan, P. Parveen, Salomi, K. Reddy
A simple, rapid, precise and accurate method is developed for the quantitative simultaneous determination of ceftriaxone and tazobactum in bulk and pharmaceutical formulations. Separation of ceftriaxone and tazobactum was successfully achieved by using Inertsil C18 ODS column 250X4.6mm, 5µm in an isocratic mode using water and acetonitrile (80:20) at a flow rate of 1.0 ml/min and was monitored at 254 nm with a retention time of 3.049 minutes and 4.317 minutes for ceftriaxone and tazobactum respectively. The method was validated and the response was found to be linear in the drug concentration range of 20µg/ml to 80 µg/ml for ceftriaxone and 5 µg/ml to 35 µg/ml for tazobactum. The values of the correlation coefficient were found to be 0.999 for ceftriaxone and 0.999 for tazobactum respectively. The LOD and LOQ for ceftriaxone were found to be 0.021 and 0.064 respectively. The LOD and LOQ for tazobactum were found to be 0.030 and 0.091 respectively. The percentage recovery for ceftriaxone and tazobactum were found to be 98-102% respectively which indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample. The method was extensively validated according to ICH guidelines for Linearity, Accuracy, Precision, Specificity and Robustness.  Stability of the drugs was determined by using acid/base, thermal, oxidative stress testing.
建立了一种简便、快速、精确、准确的同时定量测定原料药和制剂中头孢曲松和他唑巴坦含量的方法。采用Inertsil C18 ODS色谱柱250X4.6mm, 5µm,水和乙腈(80:20),流速为1.0 ml/min,在254 nm处监测,头孢曲松和他唑巴坦的保留时间分别为3.049 min和4.317 min,成功分离头孢曲松和他唑巴坦。结果表明,头孢曲松在20µg/ml ~ 80µg/ml范围内、他唑巴坦在5µg/ml ~ 35µg/ml范围内呈线性关系。头孢曲松和他唑乳的相关系数分别为0.999和0.999。头孢曲松的定量限和定量限分别为0.021和0.064。结果表明,该方法的定量限和定量限分别为0.030和0.091。头孢曲松和他唑巴坦的回收率分别为98 ~ 102%,表明该方法具有较高的准确度。该方法的特异性表明,标准品的保留时间与样品的保留时间具有良好的相关性。根据ICH指南对该方法进行了线性、准确度、精密度、特异性和鲁棒性的广泛验证。采用酸/碱、热、氧化应激等测试方法测定药物的稳定性。
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引用次数: 0
Development and validation of new analytical method for the simultaneous estimation of omeprazole and domperidone in pharmaceutical dosage form by UV spectrophotometry 紫外分光光度法同时测定药品剂型中奥美拉唑和多潘立酮含量的新方法的建立与验证
Pub Date : 2019-04-15 DOI: 10.33974/ijrpca.v1i2.63
V. P. Kumar, C. Chandra, N. Devendra, M. K. Kumar, S. R. Basha, C. S. Kumar, B. S. Naidu
A simple, rapid and precise method was developed for the quantitative simultaneous determination of Omeprazole and Domperidone in combined pharmaceutical-dosage forms. The method was based on UV-Spectrophotometric determination of two drugs, using simultaneous equation method. It involves absorbance measurement at 291 nm (λmax of Omeprazole) and 289 nm (λmax of Domperidone) in Methanol: Acetonitrile (30:70 v/v). For UV Spectrophotometric method, linearity was obtained in concentration range of 1-15 µg/ml for Domperidone and 1-50 µg/ml for Omeprazole respectively, with regression 0.999 and 0.999 for Domperidone and Omeprazole respectively. Recovery was in the range of 99 -103%; the value of standard deviation and %R.S.D were found to be < 2 %; shows the high precision of the method., in accordance with ICH guidelines. The method has been successively applied to pharmaceutical formulation and was validated according to ICH guidelines.
建立了一种简便、快速、准确的同时定量测定复方奥美拉唑和多潘立酮含量的方法。本方法以紫外分光光度法测定两种药物为基础,采用联立方程法。在甲醇:乙腈(30:70 v/v)中,在291 nm(奥美拉唑的λmax)和289 nm(多潘立酮的λmax)处进行吸光度测量。紫外分光光度法在多潘立酮1 ~ 15µg/ml、奥美拉唑1 ~ 50µg/ml浓度范围内线性良好,多潘立酮和奥美拉唑的回归分别为0.999和0.999。回收率为99 ~ 103%;标准偏差和% rs的值D < 2%;表明该方法具有较高的精度。,符合ICH指南。该方法已先后应用于药物制剂,并根据ICH指南进行了验证。
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引用次数: 0
Development and validation of new analytical method for the estimation of fluoxetine in bulk and dosage form by UV spectrophotometry 紫外分光光度法测定氟西汀原料药和剂型的新分析方法的建立与验证
Pub Date : 2019-03-27 DOI: 10.33974/ijrpca.v1i2.54
Uday sankar raju K, Vimalakkannan T, K. Ravindra Reddy, P. Naveena, R. Riharika raj, S. Chinna subbarayudu, T. Hima bindu
A simple, rapid and precise method is developed for the quantitative determination of Fluoxetine in combined pharmaceutical-dosage forms. The method was based on UV Spectrophotometric determination of Fluoxetine drug using Beer-Lamberts Law. It involves absorbance measurement at 224 nm (λmax of Fluoxetine) in water. For UV Spectrophotometric method, linearity was obtained in concentration range of 5-30 mcg/ml with regression 0.999 for Fluoxetine respectively. Recovery was in the range of 98 -102%; the value of standard deviation and %R.S.D was found to be < 2 shows high precision of the method..
建立了一种简便、快速、准确的测定复方氟西汀含量的方法。建立了用比尔-兰伯特定律紫外分光光度法测定氟西汀的方法。它涉及在224 nm(氟西汀的λmax)水中的吸光度测量。紫外分光光度法测定氟西汀浓度在5 ~ 30 mcg/ml范围内线性良好,回归系数为0.999。回收率在98 ~ 102%之间;标准偏差和% rs的值发现D < 2表明该方法精度高。
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引用次数: 1
期刊
International Journal of Research In Pharmaceutical Chemistry and Analysis
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