Management of validation of HPLC method for determination of acetylsalicylic acid impurities in a new pharmaceutical product.
Management of validation of HPLC method for determination of acetylsalicylic acid impurities in a new pharmaceutical product.
复制标题
用于测定新药中乙酰水杨酸杂质的HPLC方法验证的管理。
DOI：
10.1038/s41598-021-99269-x
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发表时间：
2022-01-06
影响因子：
4.6
通讯作者：
Turek P
中科院分区：
文献类型：
--
作者：
Kowalska M;Woźniak M;Kijek M;Mitrosz P;Szakiel J;Turek P
本工作主要侧重于对新制剂-片剂中水杨酸和单个未知杂质含量的测定方法进行验证，片剂含：75、100或150 mg乙酰水杨酸和甘氨酸，每剂40 mg。采用高效液相色谱法，以沃茨Symmetry C18色谱柱（4.6 × 250 mm，5 μm）为固定相进行分离。移动的相由85%正磷酸、乙腈和纯化水（2：400：600 V/V/V）的混合物组成。在237 nm波长下进行检测，恒定流速为1.0 ml min-1。为了验证该方法，测定了线性、精密度（重复性和重现性）、准确度、专属性、范围、耐用性、系统精密度、供试品和标准品溶液的稳定性、定量限和强制降解。根据ICH（人用药品注册技术要求国际协调会议）指导原则进行验证试验。该方法已成功验证。经证实，在0.005-0.40%水杨酸（相对于乙酰水杨酸含量）的检测范围内，该方法具有线性、精密度和准确度。
The work mainly focused on a validation of the method for determining the content of salicylic acid and individual unknown impurities in new pharmaceutical product—tablets containing: 75, 100 or 150 mg of acetylsalicylic acid and glycine in the amount of 40 mg for each dosage. The separation of the components was carried out by means of HPLC, using a Waters Symmetry C18 column (4.6 × 250 mm, 5 μm) as the stationary phase. The mobile phase consisted of a mixture of 85% orthophosphoric acid, acetonitrile and purified water (2:400:600 V/V/V). Detection was carried out at a wavelength of 237 nm, with a constant flow rate of 1.0 ml min−1. In order to verify the method, linearity, precision (repeatability and reproducibility), accuracy, specificity, range, robustness, system precision, stability of the test and standard solution, limit of quantification and forced degradation were determined. Validation tests were performed in accordance with ICH (International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use) guidelines. The method was validated successfully. It was confirmed that the method in a tested range of 0.005–0.40% salicylic acid with respect to acetylsalicylic acid content is linear, precise and accurate.
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影响因子：
8.8
作者：
Blessy M;Patel RD;Prajapati PN;Agrawal YK
通讯作者：
Agrawal YK
影响因子：
--
作者：
Busse, W
通讯作者：
Busse, W
影响因子：
3.8
作者：
Kusche, W;Paxinos, R;Breddin, HK
通讯作者：
Breddin, HK
影响因子：
0.8
作者：
Yenduri, Gopikrishna;Navuluri, Srinivasu
通讯作者：
Navuluri, Srinivasu
DOI：
10.1016/j.jpba.2005.04.008
发表时间：
2005-09-15
影响因子：
3.4
作者：
Zakeri-Milani, P;Barzegar-Jalali, M;Valizadeh, H
通讯作者：
Valizadeh, H