The Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing, China.
National Institute for the Control of Pharmaceutical and Biological Products, Beijing, China.
J Pharm Pharmacol. 2019 Dec;71(12):1864-1870. doi: 10.1111/jphp.13152. Epub 2019 Sep 5.
This study aimed to develop an efficient and reliable method for estimating common adulterants in saffron by detecting their characteristic components to warrant its efficacy and regular use as a highly valuable medicinal herb.
A selective and sensitive high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) method was developed to estimate the common adulterants in saffron from corn stigma, chrysanthemum and safflower through the simultaneous determination of specific constituents including allantoin, chlorogenic acid (ChA) and hydroxysafflor yellow A (HSYA). Peak identification of each target compound was confirmed from product ions obtained using multiple reaction monitoring triggered enhanced product ions mass chromatogram. Method validation in terms of linearity, sensitivity, reproducibility, accuracy and stability was systematically performed according to official guidelines.
Satisfactory separation of the three components was achieved on a C column (4.6 × 250 mm, 5 μm) with methanol-acetonitrile-ammonium acetate (3.0 mm) as the mobile phase at gradient elution. The identification of these specific constituents was accomplished using the multiple reaction monitoring mode in combination with enhanced product ion supplementary confirmation. The established method was validated in terms of linearity, sensitivity, reproducibility, accuracy and recovery, which were found satisfactory for sensitive detection of the three target compounds.
By detecting the specific constituents allantoin, ChA and HSYA in one run, the adulterants of corn stigma, chrysanthemum and safflower can be effectively identified and estimated in saffron. This is the first report on developing a simple, sensitive and operational method for the identification and estimation of common adulterants of saffron, that was forwarded for broaden application.
本研究旨在开发一种高效可靠的方法，通过检测其特征成分来估算藏红花中的常见掺杂物，以保证其功效和作为一种极具价值的药用植物的常规使用。
建立了一种选择性和灵敏的高效液相色谱-串联质谱（HPLC-MS/MS）方法，通过同时测定包括尿囊素、绿原酸（ChA）和羟基红花黄色 A（HSYA）在内的特定成分来估算藏红花中来自玉米须、菊花和红花的常见掺杂物。通过使用多重反应监测触发增强产物离子质量色谱图获得的产物离子对每个目标化合物的峰进行鉴定。根据官方指南，系统地进行了线性、灵敏度、重现性、准确性和稳定性方面的方法验证。
在 C 柱（4.6×250mm，5μm）上，以甲醇-乙腈-乙酸铵（3.0mm）为流动相，采用梯度洗脱，实现了三种成分的良好分离。使用多重反应监测模式结合增强产物离子补充确认完成了这些特定成分的鉴定。该方法在线性、灵敏度、重现性、准确性和回收率方面进行了验证，结果表明该方法对三种目标化合物的灵敏检测令人满意。
通过在一次运行中检测尿囊素、ChA 和 HSYA 等特定成分，可以有效识别和估算藏红花中的玉米须、菊花和红花等掺杂物。这是首次报道建立一种简单、灵敏和可操作的方法来识别和估算藏红花的常见掺杂物，该方法具有广泛的应用前景。
