近红外光谱法快速测定附子中总灰分、酸不溶性灰分和胆巴残留  

Rapid determination of total ash,acid insoluble ash and Danba residue in Radix Aconiti Lateralis Praeparata based on near infrared spectroscopy

作　　者：戴胜云 蒋双慧 高妍 刘杰[1] 乔菲[1] 过立农[1] 马双成[1] 郑健[1] DAI Sheng-yun;JIANG Shuang-hui;GAO Yan;LIU Jie;QIAO Fei;GUO Li-nong;MA Shuang-cheng;ZHENG Jian(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2022年第10期1856-1863,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会2020国家药品标准提高—制川乌制草乌标准提高研究(2020Z008);中国食品药品检定研究院中青年基金项目(2021022A2)。

摘　　要：目的:采用近红外光谱法快速分析附子中的总灰分、酸不溶性灰分和胆巴残留。方法:选择40批附子,包括白附片、黑顺片和生附片,样品粉碎后,采用漫反射的方式采集样品近红外光谱(NIRS),扫描范围1950~1550 cm^(-1),扫描次数32,分辨率16 cm^(-1),温度(25±2)℃,相对湿度(55±2)%,每份样品重复测定3次。按照2020年版《中华人民共和国药典》通则中总灰分测定法及酸不溶性灰分测定40批样品的总灰分和酸不溶性灰分,通过化学法测定胆巴残留。用Kenston样本集划分方法划分数据集,其中26批附子样品为校正集,其余14批为验证集,建立总灰分、酸不溶性灰分和胆巴残留与NIR光谱数据之间的偏最小二乘法(PLS)模型。结果:测得的样品的总灰分为1.40%~15.4%,酸不溶性灰分为0.008%~0.812%,胆巴残留为0.044%~1.464%。所建立的PLS模型中,总灰分、酸不溶性灰分和胆巴残留模型的相对预测偏差(RPD)分别为5.17、3.47和3.41,验证集相关系数(r_(pre))分别为0.9821,0.9780和0.9750,说明NIRS模型验证集与总灰分、酸不溶性灰分和胆巴残留测定值具有良好的线性关系,模型预测效果良好。结论:采用NIRS技术结合PLS模型可以快速对附子中的总灰分、酸不溶性灰分和胆巴残留进行测定,方法操作简便,对控制附子质量有一定的指导作用。Objective:To establish a rapid determination method for the total ash,acid insoluble ash and Danba residue in Aconiti Lateralis Radix Praeparata by near infrared spectroscopy(NIRS).Methods:40 batches of samples were selected,including Baifu Pian,Heishun Pian and Shengfu Pian.After the samples were crushed,the near infrared spectra(NIRS)of the samples were collected by diffuse reflection.The scanning range was 1950-1550 cm-1,the scanning times were 32,the resolution was 16 cm-1,the temperature was(25±2)℃,the relative humidity was(55±2)%,and each sample was scanned for 3 times.According to the general principles of Chinese Pharmacopoeia 2020,total ash and acid insoluble ash were determined,and the Danba residue was determined by chemical method.Kenston division method was used to divide the data set,of which 26 batches of samples were selected in the calibration set,and the remaining 14 batches were selected in the validation set.Partial least squares(PLS)models between total ash,acid insoluble ash,Danba residue and NIR spectral data were established.Results:The determination results of total ash,acid insoluble ash and Danba residue were 1.40%-15.4%,0.008%-0.812%,and 0.044%-1.464%,respectively.The relative prediction deviation(RPD)of the total ash,acid insoluble ash and Danba residue models were 5.17,3.47 and 3.41 respectively,and the correlation coefficient(r_(pre))of the validation set were 0.9821,0.9780 and 0.9750 respectively,indicating the predicted values of NIRS model and the measured values showed a good linear relation.Conclusion:The method of NIRS combined with PLS model can be used to quickly determine the total ash,acid insoluble ash and Danba residue in Aconiti Lateralis Radix Praeparata.The method is simple and has a certain guiding role in controlling the quality of Aconiti Lateralis Radix Praeparata.

关 键 词：近红外光谱法 附子 总灰分 酸不溶性灰分 胆巴残留量 偏最小二乘法 

分 类 号：R917[医药卫生—药物分析学]