Objective: To establish a remote and fast near-infrared spectrum(NIRS) quantitative model of duloxetine hydrochloride particle size, and to provide a real-time monitoring system for the production of duloxetine hydrochloride tablets. Methods: The NIRS spectra of duloxetine hydrochloride granules samples were collected and the reference values were determined by laser particle size analyzer. The pretreatment method of constant spectrum and no smoothing was selected. The modeling band was 5 550.00-7 400.00 cm-1. The model was established by partial least square method. The model was used to predict the independent sample sets of different batches, and the results were verified by laser particle size analyzer. Results: The root mean square error of the model was 0.005 9, the correlation coefficient rC was 0.965 7, the root mean square error of prediction was 0.007 3, the correlation coefficient rP was 0.946 5, and the ratio of prediction to deviation was 3.85. The prediction error of the model for other batch of independent sample set is less than 5%. Conclusion: The quantitative model of duloxetine hydrochloride granules based on NIR spectrum can predict the particle size immediately and accurately, which provides a feasible path for online real-time monitoring of the particle size of preparation and stable uniformity of produced drugs.
[1] 吴志生, 杜敏, 潘晓宁, 等.粒径对多类中药材NIR频谱区的检测研究[J].中国中药杂志, 2015, 40 (2):287
WU ZS, DU M, PAN XN, et al. Detection of particle size in NIR spectrum region of many kinds of Chinese medicinal materials [J].China J Chin Mater Med, 2015, 40 (2):287
[2] 王新基, 郭涛, 潘发明, 等.利用近红外光谱技术快速分析全株玉米青贮营养成分[J].家畜生态学报, 2021, 42 (1):52
WANG XJ, GUO T, PAN FM, et al. Rapid analysis of nutrient components of whole corn silage by near infrared spectroscopy [J].J Domest Anim Ecol, 2021, 42 (1):52
[3] 王艳斌, 郭庆洲, 陆婉珍, 等.近红外分析方法测定润滑油基础油的化学族组成[J].石油化工, 2001 (3):224
WANG YB, GUO QZ, LU WZ, et al. Determination of chemical group composition of lube base oil by near infrared spectroscopy [J].Petrochem Technol, 2001 (3):224
[4] 张帆, 耿响, 李毛英, 等.基于近红外光谱法的棉/氨纶混纺织物纤维含量快速检测研究[J].红外, 2021, 42 (1):38
ZHANG F, GENG X, LI MY, et al. Fast determination of fiber content of cotton/spandex blended fabric based on near infrared spectroscopy [J].Infrared, 2021, 42 (1):38
[5] 赵科文, 陈实, 蒋浩,等.基于近红外光谱技术的烟丝掺配均匀度测定[J].食品与机械, 2020, 36 (11):183
ZHAO KW, CHEN S, JIANG H, et al. Determination of cut tobacco blending uniformity based on near infrared spectroscopy [J].Food Mach, 2020, 36 (11):183
[6] 曾敬其, 张静, 张芳语, 等.中药大品种制造关键质量属性表征:沸腾时间状态属性的提取过程在线NIR质量控制研究[J].中国中药杂志, 2021, 46 (7):1644
ZENG JQ, ZHANG J, ZHANG FY, et al. Characterization of key quality attributes in large variety manufacturing of traditional Chinese medicine: online NIR quality control of boiling time state attributes extraction process [J].China J Chin Mater Med, 2021, 46 (7):1644
[7] 张芳语, 林玲, 曾敬其, 等.中药大品种制造关键质量属性表征:空间分布均匀度质量属性的同仁牛黄清心丸贵细药混合过程控制可视化方法研究[J].中国中药杂志, 2021, 46(7):1585
ZHANG FY, LIN L, ZENG JQ, et al. Characterization of key quality attributes of large variety manufacturing of traditional Chinese medicine: study on visualization method of quality attributes of spatial distribution uniformity of Tongren Niuhuang qingxin pill in the mixing process of noble and fine drugs[J].China J Chin Mater Med, 2021, 46(7):1585
[8] 魏宇楠, 黄兴国, 曾敬其, 等.中药大品种制造关键质量属性表征:水分含量化学属性的同仁牛黄清心丸NIR现场检测方法研究[J].中国中药杂志, 2021, 46(7):1592
WEI YN, HUANG XG, ZENG JQ, et al. Characterization of key quality attributes of large varieties of Chinese medicine manufacturing: study on the NIR method of Tongren Niuhuang Qingxin Pills for the chemical properties of water content[J].China J Chin Mater Med, 2021, 46(7):1592
[9] 刘伟, 何勇, 吴斌, 等.过程分析技术(PAT)在原料药生产中的应用[J].分析测试学报, 2020, 39 (10):1239
LIU W, HE Y, WU B, et al. Application of process analysis technology in API production [J].J Instrum Anal, 2020, 39 (10):1239
[10] 郭洁, 解亚娟, 李惠, 等.近红外光谱法对脑心通胶囊药粉混合均匀度在线检测的应用[J].临床医药文献电子杂志, 2020, 7 (43):125
GUO J, XIE YJ, LI H, et al. Application of near infrared spectroscopy in online detection of mixing uniform degree of Naoxintong capsule powder [J].J Clin Med Lit, 2020, 7 (43):125
[11] 杨培.流化床制粒过程小试水分近红外定量模型向中试传递方法研究[D].北京:北京中医药大学, 2020
YANG P. Study on Transfer Method of Water From Small Scale Near Infrared Quantitative Model to Pilot Scale in Fluidized Bed Granulation Process [D].Beijing:Beijing University of Chinese Medicine, 2020
[12] 鲍斌斌.片剂生产工艺常见问题分析及解决办法[J].黑龙江科学, 2020, 11(20):43
BAO BB.Analysis and solution of common problems in tablet manufacturing process[J].Heilongjiang Sci, 2020, 11(20):43
[13] PAULI V, ROGGO Y, KLEINEBUDDE P, et al. Real-time monitoring of particle size distribution in a continuous granulation and drying process by near infrared spectroscopy [J].Eur J Pharm Biopharm, 2019, 141:90
[14] OTSUKA M, KOYAMA A, HATTORI Y. Real-time release monitoring for water content and mean particle size of granules in lab-sized fluid-bed granulator by near-infrared spectroscopy [J].RSC Adv, 2014, 4(34):17461
[15] CHEN Y, XIE M, ZHANG H, et al. Quantification of total polysaccharides and triterpenoids in Ganoderma lucidum and Ganoderma atrum by near infrared spectroscopy and chemometrics[J].Food Chem, 2012, 135(1):268
[16] 李沙沙, 陈辉, 赵云丽, 等.硫酸羟氯喹颗粒水分含量测定近红外定量模型的建立[J].沈阳药科大学学报, 2019, 36 (7):593
LI SS, CHEN H, ZHAO YL, et al. Establishment of near infrared quantitative model for determination of moisture content of hydroxychloroquine sulfate granules [J].J Shenyang Pharm Univ, 2019, 36 (7):593
[17] MI JR, ZHANG LD, ZHAO LL, et al. Particle size regression correction for NIR spectrum based on the relationship between absorbance and particle size[J].Front Optoelectron, 2013, 6 (2):216
