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Preparation of a reserpine certified reference material for calibration and analysis of liquid chromatography

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Abstract

A certified reference material (CRM) for reserpine was investigated by raw material purification, qualitative analysis, quantitative analysis, homogeneity testing, stability testing, characterization, and uncertainty evaluation. The candidate reference material was prepared by recrystallization of purchased reserpine. After purification and drying, the candidate materials were enclosed in brown glass bottles. The chemical composition of the candidate reserpine reference material was confirmed by infrared spectroscopy, high-resolution mass spectrometry, and nuclear magnetic resonance. The homogeneity and stability of several sample bottles of the candidates were studied by stratified random sampling. With the cooperation of eight qualified laboratories, the purity of reserpine was analyzed by a mass balance method (including area normalization, water content, ash content and residual solvent analyses by liquid chromatography) with a certified purity mass fraction of 99.3 % and an expanded uncertainty of 0.5 % (k = 2). This reference material has been identified as a Chinese national-grade secondary CRM, which is numbered GBW(E) 090901, and is expected to be used in the calibration of instruments such as those used for liquid chromatography or method evaluations in food, medicine, environmental, and cosmetic analyses.

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Abbreviations

LC:

Liquid chromatography

LC–MS:

Liquid chromatography–mass spectrometry

CRMs:

Certified reference materials

RMs:

Reference materials

LC-PAD:

LC with photodiode array detection

FTIR:

Fourier transform infrared spectroscopy

NMR:

Nuclear magnetic resonance

GC:

Gas chromatography

IC:

Ion chromatograph

KBr:

Potassium bromide

DTGS:

Deuterated triglycine sulfate

HS:

Headspace

SDBS:

Spectral database for organic compounds

\(\nu_{1}\) :

Intergroup degrees of freedom

\(\nu_{2}\) :

Intragroup degrees of freedom

\(\alpha\) :

Significance level

\(F_{\alpha } (\nu_{1} ,\nu_{2} )\) :

Critical value of F with \(\nu_{1}\) and \(\nu_{2}\)

\(S_{1}^{2}\) :

Square of the intergroup

\(S_{2}^{2}\) :

Square of the intragroup

\(Q_{1}\) :

SD square of the intergroup

\(Q_{2}\) :

SD square of the intragroup

\(b_{1}\) :

Slope of the fitting curve of the stability data

\(t_{0.95,n - 2}\) :

t Factor with a 95 % confidence level, a degree of n − 2

\(s(b_{1} )\) :

Standard deviation of b1

\(x_{d}\) :

Outlier with the maximum residual

\(\overline{x}\) :

Average value of eight laboratories

\(s\) :

Standard deviation of the average value

\(G(\alpha ,n)\) :

Grubbs threshold associated with the significance level and repeated observation

\(C\) :

Cochran’s factor

\(s_{\rm max}\) :

Max of \(s_{i}\)

\(s_{i}\) :

Standard deviation

\(C(0.05,8,3)\) :

Critical Cochran’s factor

\(W_{\text{LC}}\) :

Average purity determined by LC in eight laboratories

\(\sum {c_{i} }\) :

Total content of common inorganic elements (μg/L)

\(\sum {w_{i} }\) :

Total mass percentage of common inorganic elements (%)

m :

Mass of the sample, 10 mg in the test

V :

Volume of the sample, 10 mL in the test

W :

Final purity

\(s_{r}\) :

Standard deviation of the intergroup by eight laboratories

\(s_{L}\) :

Standard deviation of the intragroup by eight laboratories

\({\text{MS}}_{\text{within}}\) :

Mean square of the intergroup

\(MS_{among}\) :

Mean square of the intragroup

n :

Number of tests

p :

Number of laboratories

\(u_{\text{LC}}\) :

Uncertainty of eight laboratories’ collaborative characterization with LC

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Acknowledgements

The authors acknowledge the support from the Technical Project of Guangdong Provincial Bureau of Quality and Technical Supervision (2013ZJ02, 2016CJ03, 2018ZJ02), the Technical Project of Guangdong Science and Technology Department (2017A040405034) and the National Natural Science Foundation of China (NSFC) Grant 21204001. The valuable suggestion from Dr. Yan Guan at the College of Chemistry and Molecular Engineering, Peking University, is sincerely appreciated.

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Authors and Affiliations

  1. Guangdong Provincial Institute of Metrology, South China National Centre of Metrology, Guangzhou, China

    Jinyan Zhou, Yanjie Huang, Ling Chen, Junbin Xu, Keng Lin, Yuanwen Mao & Qiang Yin

  2. Guangdong Provincial Key Laboratory of Modern Geometric and Mechanical Metrology Technology, Guangzhou, China

    Jinyan Zhou, Ling Chen, Junbin Xu & Qiang Yin

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  1. Jinyan Zhou
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  2. Yanjie Huang
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  3. Ling Chen
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  4. Junbin Xu
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  5. Keng Lin
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  6. Yuanwen Mao
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  7. Qiang Yin
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Correspondence to Yanjie Huang.

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Zhou, J., Huang, Y., Chen, L. et al. Preparation of a reserpine certified reference material for calibration and analysis of liquid chromatography. Accred Qual Assur 25, 51–60 (2020). https://doi.org/10.1007/s00769-019-01412-9

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