Bioanlytical Research, Bristol Myers-Squibb, Chicago, Illinois, USA.
J Agric Food Chem. 2009 Nov 11;57(21):10014-21. doi: 10.1021/jf9020224.
Dietary supplements containing preparations of ginger roots/rhizomes (Zingiber officinale Roscoe) are being used by consumers, and clinical trials using ginger dietary supplements have been carried out to evaluate their anti-inflammatory or antiemetic properties with inconsistent results. Chemical standardization of these products is needed for quality control and to facilitate the design of clinical trials and the evaluation of data from these studies. To address this issue, methods based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) were developed for the detection, characterization, and quantitative analysis of gingerol-related compounds in botanical dietary supplements containing ginger roots/rhizomes. During negative ion electrospray with collision-induced dissociation, the cleavage of the C4-C5 bond with a neutral loss of 194 u and benzylic cleavage leading to the neutral loss of 136 u were found to be class-characteristic fragmentation patterns of the pharmacologically active gingerols or shogaols, respectively. On the basis of these results, an assay using LC-MS/MS with neutral loss scanning (loss of 194 or 136 u) was developed that is suitable for the fingerprinting of ginger dietary supplements based on the selective detection of gingerols, shogaols, paradols, and gingerdiones. In addition, a quantitative assay based on LC-MS/MS with selected reaction monitoring was developed for the quantitative analysis of 6-gingerol, 8-gingerol, 10-gingerol, 6-shogaol, 8-shogaol, and 10-shogaol in ginger dietary supplements. After method validation, the quantities of these compounds in three commercially available ginger dietary supplements were determined. This assay showed excellent sensitivity, accuracy, and precision and may be used to address the need for quality control and standardization of ginger dietary supplements.
消费者正在使用含有姜根茎(姜黄)制剂的膳食补充剂,并且已经进行了使用姜膳食补充剂的临床试验,以评估其抗炎或止吐特性,但结果不一致。为了进行质量控制并促进临床试验的设计和这些研究数据的评估,需要对这些产品进行化学标准化。为了解决这个问题,开发了基于液相色谱-串联质谱(LC-MS/MS)的方法,用于检测、表征和定量分析含有姜根茎的植物性膳食补充剂中的姜酚相关化合物。在负离子电喷雾与碰撞诱导解离过程中,发现具有中性损失 194 u 的 C4-C5 键的裂解和导致中性损失 136 u 的苄基裂解分别是具有药理活性的姜酚或姜烯酚的特征性裂解模式。基于这些结果,开发了一种使用 LC-MS/MS 进行中性损失扫描(损失 194 或 136 u)的测定方法,该方法适合基于姜酚、姜烯酚、姜二醇和姜二酮的选择性检测对姜膳食补充剂进行指纹分析。此外,还开发了一种基于 LC-MS/MS 选择反应监测的定量分析方法,用于定量分析姜膳食补充剂中的 6-姜酚、8-姜酚、10-姜酚、6-姜烯酚、8-姜烯酚和 10-姜烯酚。在方法验证后,确定了三种市售姜膳食补充剂中这些化合物的含量。该测定方法具有出色的灵敏度、准确性和精密度,可用于满足姜膳食补充剂的质量控制和标准化需求。