Simultaneous Quantification of Six Bioactive Components in Decoction of Ziziphi spinosae Semen Using Ultrahigh Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry.

Xiao Liu,Jia Ma,Baochang Cai,Yinghui Xu,Hui Zhu,Zejun Wu,Qigang Zhou,Li Xie,Xiaochai Zhu

doi:10.1155/2018/8397818

Abstract

This paper was conducted to develop a method containing ultrahigh performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry for simultaneous quantification of six bioactive components in the decoction of Ziziphi spinosae Semen. Analysis was performed on an Agilent ZORBAX Extend-C18 column (2.1 × 100 mm, 1.8 μm) and eluted with a mobile phase system consisting of acetonitrile and water under a gradient program with a flow rate of 0.3 ml/min. The injection volume was 2 μl. Multiple-reaction monitoring scanning detection was employed for quantification with an electrospray ion source in the negative ion mode. All the six compounds showed good linearities (r ≥ 0.9996). The LODs of the six bioactive compounds were 0.039 ng/ml, 0.092 ng/ml, 3.112 ng/ml, 2.131 ng/ml, 0.099 ng/ml, and 0.071 ng/ml for spinosin, 6‴-feruloylspinosin, jujuboside A, jujuboside B, camelliaside B, and betulinic acid, respectively. The LOQs were 0.118 ng/ml, 0.276 ng/ml, 9.336 ng/ml, 6.393 ng/ml, 0.299 ng/ml, and 0.213 ng/ml for spinosin, 6‴-feruloylspinosin, jujuboside A, jujuboside B, camelliaside B, and betulinic acid, respectively. According to our knowledge, it was the first time to establish a method with high efficiency and accuracy for the quantification of six bioactive components in the decoction of Ziziphi spinosae Semen, which would provide references for quality control and evaluation of Ziziphi spinosae Semen.

Highlights

Ziziphi spinosae Semen (ZSS; suanzaoren in Chinese), the seeds of Ziziphus jujuba Mill. var. spinosa (Bunge) Hu ex H
Several studies have reported the analysis of relative chemical constituents in ZSS; the limitation of the performance coming from traditional detectors, such as UV and ELSD, made it quite difficult to detect a variety of complex components in ZSS quickly and accurately [12, 13]
Chemical constituents of ZSS have been studied in some previous research studies [18, 19], but none of them could determine the contents of its active components efficiently due to the diversity of these constituents

Summary

Introduction

Ziziphi spinosae Semen (ZSS; suanzaoren in Chinese), the seeds of Ziziphus jujuba Mill. var. spinosa (Bunge) Hu ex H. E combination of tandem mass spectrometry with UHPLC made it possible for the effective and reliable detection of complex constitutions in TCM, which would compensate for the 3 shortcomings in Journal of Analytical Methods in Chemistry the previous research studies [14,15,16,17]. Organic solvents were used for sample extraction in most of the existing research studies [21], which was different from TCM actual application in clinics. This might lead to a limitation of these research studies for guiding ZSS clinical application and quality control

Experimental

Results and Discussion

Assay Validation

Conclusions