Office of Regulatory Science, Center for Food Safety and Applied Nutrition, U.S. Food and Drug Administration, College Park, MD, USA.
Drug Test Anal. 2020 Sep;12(9):1241-1251. doi: 10.1002/dta.2871. Epub 2020 Jun 28.
Citrus aurantium, commonly known as bitter orange, is a popular dietary supplement ingredient sold worldwide. Bitter orange supplements are sold primarily as weight management and sports performance products and have gained popularity after Ephedra products were banned from the US market. Supplements containing synephrine are reported to exhibit adverse cardiovascular effects especially in the presence of caffeine. In this study, an LC-MS/MS method was established to quantify five natural amines (synephrine, octopamine, tyramine, N-methyltyramine, and hordenine) and four synthetic phenethylamines (phenylephrine, methylsynephrine, etilefrine, and isopropyloctopamine) in dietary supplements sold in the US. The method was validated and found to have acceptable performance to accurately measure analytes in complex botanical products. The average recoveries from a blank matrix were 88-125% with an RSD of 0.5-7.0%. Fifty-nine products labeled to contain bitter orange peel, extract, or its amines were purchased and their amine content was measured. Several products were found to contain higher amounts of amines than that expected from a typical bitter orange extract. Of the 23 products that made label claims for synephrine, only 5 products (22%) were within 80-120% of labeled synephrine content. The presence of synthetic amines, methylsynephrine (up to 240 mg/daily serving), and isopropyloctopamine (up to 76 mg/daily serving), whose effects in humans are not known, were detected in six products and one product, respectively. While the use of methylsynephrine and isopropyloctopamine are not permitted in dietary supplements, hordenine, N-methyltyramine, and octopamine are currently listed on the FDA's Dietary Supplement Ingredient Advisory List.
酸橙，通常被称为苦橙，是一种流行的膳食补充剂成分，在全球范围内销售。苦橙补充剂主要作为体重管理和运动表现产品销售，并在美**用禁令后广受欢迎。含有辛弗林的补充剂据报道会表现出不良的心血管作用，尤其是在存在咖啡因的情况下。在这项研究中，建立了一种 LC-MS/MS 方法来定量五种天然胺（辛弗林、章鱼胺、酪胺、N-甲基酪胺和霍多宁）和四种合成苯乙胺（苯丙醇、甲基辛弗林、依替福林和异丙基辛福林）在美国销售的膳食补充剂。该方法经过验证，具有可接受的性能，可以准确测量复杂植物产品中的分析物。空白基质的平均回收率为 88-125%，RSD 为 0.5-7.0%。购买了 59 种标有含有苦橙皮、提取物或其胺的产品，并测量了它们的胺含量。发现一些产品含有比典型的苦橙提取物更高的胺。在 23 种声称含有辛弗林的产品中，只有 5 种（22%）的产品的辛弗林含量在 80-120%的标签范围内。在六种产品和一种产品中分别检测到了合成胺、甲基辛弗林（高达 240 毫克/每日剂量）和异丙基辛福林（高达 76 毫克/每日剂量），其在人体中的作用尚不清楚。虽然甲基辛弗林和异丙基辛福林在膳食补充剂中不被允许使用，但霍多宁、N-甲基酪胺和章鱼胺目前被列入 FDA 的膳食补充剂成分咨询清单。
