Simultaneous determination of 14 components in Shuanghua Baihe tablets by ultrasonic-assisted extraction and HPLC-MS/MS
Simultaneous determination of 14 components in Shuanghua Baihe tablets by ultrasonic-assisted extraction and HPLC-MS/MS
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超声辅助提取-HPLC-MS/MS同时测定双花白鹤片中14种成分
DOI：
10.1039/c6ay00143b
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发表时间：
2016-01-01
影响因子：
3.1
通讯作者：
Ma, Xiao-Chi
中科院分区：
文献类型：
--
作者：
Zheng, Lu;Huo, Xiao-Kui;Ma, Xiao-Chi
开发并验证了一种简单、灵敏、选择性和可靠的高性能液相色谱-串联质谱 (HPLC-MS/MS) 方法，可同时检测和定量 14 种化合物。这些化合物在 Kinetex C18 核壳柱上以乙腈和 0.1% 甲酸为流动相在 13 分钟内完全分离。该柱与同时在正离子和负离子模式下操作的 ESI 三重四极杆质谱仪耦合。在多重反应监测采集模式下总共对 14 种成分进行了定量。这些化合物的检测限范围为 0.12 至 2.10 ng mL−1，而定量限范围为 0.40 至 7.09 ng mL−1。所有校准曲线在测试范围内均表现出良好的线性（r > 0.999）。还使用正交设计实验来研究提取变量（包括温度、甲醇与水的比例百分比和超声处理时间）对超声辅助提取（UAE）的影响。最佳提取条件和经过验证的方法已成功用于分析从中国市场购买的 10 批双花白鹤片 (SBT)。经验证，该方法简单、快速、准确、可靠，可同时测定SBT中的14种成分，结果为SBT质量的整体评估提供了新的依据。
A simple, sensitive, selective, and reliable high-performance liquid chromatograph-tandem mass spectrometry (HPLC-MS/MS) method was developed and validated for the simultaneous detection and quantification of 14 compounds. These compounds were separated completely within 13 min on a Kinetex C18 core–shell column with acetonitrile and 0.1% formic acid as the mobile phase. The column was coupled to an ESI-triple-quadrupole mass spectrometer operated in positive and negative ion mode simultaneously. In total, 14 components were quantified in multiple reactions monitoring acquisition mode. The limits of detection of these compounds ranged from 0.12 to 2.10 ng mL−1, whereas the limits of quantitation ranged from 0.40 to 7.09 ng mL−1. All the calibration curves showed good linearities (r > 0.999) within the test ranges. An orthogonal design experiment was also used to investigate the effect of the extraction variables, including temperature, methanol to water ratio percent, and sonication time, on the ultrasound-assisted extraction (UAE). The optimum extraction condition and validated method was successfully used to analyze 10 batches of Shuanghua Baihe tablets (SBT) bought from Chinese markets. The method was validated to be simple, rapid, accurate and reliable to simultaneously determine 14 components in SBT and our results provide a new basis for the overall assessment of SBT quality.