Objective: To improve the accuracy and stability of near infrared spectroscopy (NIR) in the determination of moisture in Xiaochaihu granules, and to enhance the application value of this method. Methods: The NIR spectra matrix of Xiaochaihu granules with water contents of 1.70%, 1.80%, 1.90%, 2.00%, 2.10%, 2.20%, 2.30%, 2.40%, 2.50%, 2.60% and 2.69% were used as the EPO reconstruction matrix to reconstruct the absorbance of 9 000-4 000 cm-1 band and water characteristic spectrum band (4 980-5 140 cm-1/ 6 900-7 010 cm-1) in the NIR spectra of 420 Xiaochaihu granules. Particles and integrate multiple model evaluation indexes including model determination coefficient R2, root mean standard error of calibration(RMSEC), root mean square error of cross validation(RMSECV), the predicted standard error SEP of 60 external samples and the paired t-test results between model predicted values and measured values were used to compare the modeling effect of PLS before and after reconstruction. The precision of this method also had been investigated. Results: EPO reconstruction could significantly improve the stability and accuracy of the model. EPO and 9 000-4 000 cm-1 spectrum band had the best modeling effect, the prediction ranges of the model were 1.68%-2.69%, the optimal principal component was 8, the determination coefficient R2 was 0.938, and the RMSEC and RMSECV were 0.042 9% and 0.047 6%, respectively. The prediction standard error SEP of the external validation set was 5.18%. There was no significant difference between the measured values and model predictive values of 60 validation sets at α=0.05 confidence level. The intra-day precision of the three batches of samples with different moisture contents was between 1.33% and 1.54%, and the inter-day precision was between 2.08% and 2.21%. Conclusion: EPO reconstruction can significantly improve the stability and accuracy of Xiaochaihu granules moisture NIR calibration model. This research provides technical support for the NIR application in the rapid determination of Xiaochaihu granules moisture.
LIU Jing, ZHANG Yan, WANG Li-fang, ZAHNG Tao, XIANG Wan, ZHOU Wen-zhong, YANG Xiao-yun, YANG Pan-pan
. Determination of moisture in Xiaochaihu granules by EPO-PLS based on near infrared spectroscopy*[J]. Chinese Journal of Pharmaceutical Analysis, 2023
, 43(5)
: 827
-836
.
DOI: 10.16155/j.0254-1793.2023.05.13
[1] 杨安辉,石国琳,刘宇灵,等. 多变量分析模型在固体制剂全过程控制的应用[J].中国中药杂志,2022, 47(14):3701
YANG AH,SHI GL, LIU YL, et al. Application of multivariate analysis model in the whole process control of solid preparation[J].China J Chin Mater Med, 2022, 47(14):3701
[2] 刘南岑,耿立冬,马丽娟,等. 中药制造领域近红外光谱技术的专利技术进展和趋势[J].中草药,2021,52(21):6768
LIU NC, GENG LD, MA LJ, et al. Patent technology progress and trend of near-infrared spectroscopy technology in traditional Chinese medicine manufacturing[J].Chin Tradit Herb Drugs, 2021, 52(21):6768
[3] 赵瑜,朱俐,尹利辉. 近红外光谱法分析头孢拉定颗粒的关键质量属性及对其量值的测定[J].中国抗生素杂志,2022,47(2):203
ZHAO Y, ZHU L, YIN LH. Analysis of the critical quality attributes of cefradine granules and determination of their quantity by near-infrared spectroscopy[J]. Chin J Antibiot, 2022, 47(2):203
[4] 曲正义,逄世峰,王兆森,等. 基于近红外光谱技术的大力参含水量快速无损检测[J].时珍国医国药,2020,31(11):2653
QU ZY, PANG SF, WANG ZS, et al. Rapid nondestructive testing of water content in Radix Ginseng based on near infrared spectroscopy[J].Lishizhen Med Mater Med Res, 2020, 31(11):2653
[5] 王晴,徐芳芳,张欣,等. 在线近红外光谱监测桂枝茯苓胶囊流化床干燥过程水分的方法研究[J].中草药,2019,50(22):5429
WANG Q, XU FF, ZHANG X, et al. Study on on-line near-infrared spectroscopic for moisture monitoring in afluidized bed drying process of Guzhi Fuling capsules[J].Chin Tradit Herb Drugs, 2019, 50(22):5429
[6] 褚小立,陈瀑,李敬岩,等. 近红外光谱分析技术的最新进展与展望[J].分析测试学报, 2020, 39(10):1181
CHU XL, CHEN P, LI JY, et al. Progresses and perspectives of near infrared spectroscopy analytical technology[J].J Instrum Anal, 2020, 39(10):1181
[7] 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 quantitative model for determination of moisture content of hydroxychloroquine sulfate particles by near infrared spectroscopy[J].J Shenyang Pharm Univ, 2019, 36(7):593
[8] ROGER JM, CHAUCHARD F, BELLON-MAUREL V. EPO-PLS external parameter orthogonalisation of PLS application to temperature-independent measurement of sugar content of intact fruits[J].Chemom Intell Lab Syst, 2003, 66(2):191
[9] 彭翔,胡丹,曾文治,等. 基于EPO-PLS回归模型的盐渍化土壤含水率高光谱反演[J].农业工程学报,2016,32(11):167
PENG X, HU D, ZENG WZ, et al. Estimating soil moisture from hyperspectra in saline soil based on EPO-PLS regression[J].Trans Chin Soc Agric Eng, 2016, 32(11):167
[10] NAWAR S, MUNNAF MA, MOUAZEN AM. Machine learning based on-line prediction of soil organic carbon after removal of soil moisture effect[J]. Remote Sens, 2020, 12(8):1308
[11] OGEN Y, FAIGENBAUM-GOLOVIN S, GRANOT A, et al. Removing moisture effect on soil reflectance properties: a case study of clay content prediction[J].Pedosphere, 2019, 29(4):421
[12] 高乐乐,钟亮,董海玲,等. 基于近红外光谱的甜菊糖吸湿过程表征及莱鲍迪苷A含量快速测定的研究[J].光谱学与光谱分析,2022,42(2):415
GAO LL, ZHONG L, DONG HL, et al. Characterization of moisture absorption process of stevia and rapid determination of rbaudioside a content by using near-infrared spectroscopy[J].Spectrosc Spect Anal, 2022, 42(2):415
[13] 刘静,胡建西,杨芳芳,等. 近红外光谱结合线性非负回归测定梗丝掺配比例[J].食品与机械,2021,37(11):188
LIU J, HU JX, YANG FF, et al. Detection of mixing proportion of stem by near infrared spectroscopy combined with linear non-negative regression coefficient regression method[J].Food Mach, 2021, 37(11):188
[14] 陆婉珍. 现代近红外光谱分析技术[M].第二版.北京:中国石化出版社,2006:39
LU WZ. Modern Near Infrared Spectroscopy Analytical Technology[M]. 2nd Ed. Beijing: China Petrochemical Press,2006:39
[15] ZHENG KY, FENG T, ZHANG W, et al. Weighted SPXYE(WSPXYE) and its application to transfer set selection in near infrared spectra[J].Spectrosc Spect Anal, 2021, 41(3):984
[16] 中华人民共和国国家质量监督检验检疫总局/中国国家标准化管理委员会. 分子光谱多元校正定量分析通则[S].2012:2
General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China/Standardization Administration of The People’s Republic Of China. Standard Guidelines for Molecular Spectroscopy Multivariate Calibration Quantitative Analysis[S].2012:2
[17] LI HD, XU QS, LIANG YZ. libPLS: an integrated library for partial least squares regression and discriminant analysis[J].Chemom Intell Lab Syst, 2018, 176:34
