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建立了超声辅助萃取-热辅助在线衍生化-气相色谱法测定银杏保健品中银杏酸的分析方法。在超声辅助下以甲醇萃取样品,分别吸取2.0μL衍生化试剂三甲基氢氧化硫(TMSH)与1.0μL萃取液先后加入裂解器进样杯,银杏酸在裂解炉300℃的高温下瞬间生成甲基化产物,由GC-FID(MS)分离测定。结果表明,银杏酸GA13:0在5~600 mg/L范围内线性良好,线性相关系数0.9994,检出限为1.8 mg/L(S/N=3),RSD为2.4%~2.6%(n=5)。以外标法分别测定白果种仁、白果粉饮品、银杏秋茶和春茶样品中的7种银杏酸,总含量在0.032~18.9 g/kg之间。同时,测定了银杏秋茶和春茶中银杏酸在冲泡90 min后的溶出率。白果粉饮品加标回收率在87.1%~106.1%之间。为银杏保健品中银杏酸的质量控制以及饮食的安全性评价提供了参考。
A method for the determination of ginkgolic acids in Ginkgo health products by ultrasonic-assisted extraction-thermal-assisted on-line derivatization-gas chromatography was established. Samples were extracted with methanol with sonication and aspirated with 2.0 μL of TMSH and 1.0 μL of extraction solution, respectively, and then added into the cracker sampling cup. Ginkgo acid was instantly generated at a high temperature of 300 ° C in a cracking furnace Methylation products were determined by GC-FID (MS) separation. The results showed that GA13: 0 showed a good linearity in the range of 5 ~ 600 mg / L with a linear correlation coefficient of 0.9994, a detection limit of 1.8 mg / L (S / N = 3) and RSD of 2.4% -2.6% = 5). The contents of seven kinds of ginkgolic acids in gingko nuts, white gingko drinks, gingko autumn tea and spring tea samples were determined by external standard method with the total contents ranging from 0.032 to 18.9 g / kg. At the same time, the dissolution rate of Ginkgo autumn tea and Ginkgo biloba in spring tea was determined after 90 min brewing. Ginkgo beverage spiked recoveries ranged from 87.1% to 106.1%. It provided a reference for the quality control of ginkgolic acids in ginkgo health products and the safety assessment of diet.