目的 運用超高效液相色譜串聯(lián)三重四極桿質(zhì)譜（HPLC-QQQ）建立一種能夠同時測定銀杏葉制劑中13個黃酮類成分的分析方法。方法 采用Agilent Poroshell 120 EC-C₁₈色譜柱（50 mm×3.0 mm，2.7 μm），以0.1%甲酸溶液-乙腈為流動相，梯度洗脫，體積流量0.3 mL/min，柱溫30℃。在電噴霧離子化負離子模式下離子化，以多反應(yīng)監(jiān)測方式（MRM）檢測。結(jié)果 13種黃酮類成分蘆丁、異槲皮苷、槲皮素-3-O-β-D-葡萄糖基（1→2）-α-L-鼠李糖苷、山柰酚-3-O-蕓香糖苷、水仙苷、槲皮苷、芹菜素-7-O-β-D-吡喃葡萄糖苷、木犀草素、槲皮素、芹菜素、山柰酚、異鼠李素、芫花素的分離度良好，在各自的質(zhì)量濃度范圍內(nèi)的線性關(guān)系良好（r=0.999 0），且精密度試驗、重復性試驗的RSD值均小于3.5%，供試品溶液在12 h內(nèi)穩(wěn)定性好，各成分的平均回收率在94.5%~100.5%。不同批次樣品之間，總黃酮含量相差不大；各批次的銀杏黃酮類成分含量均不相同，差異較大，其中黃酮苷類化合物所占比例相對較大，蘆丁、水仙苷含量均較單糖（異槲皮苷、槲皮苷）含量高，芫花素、木犀草素等黃酮苷元含量最低。結(jié)論 方法分離度好、操作簡便、專屬性強，能夠明確反映出銀杏葉提取物中13個黃酮類成分的分布和差異，可用于銀杏葉提取物制劑的質(zhì)量控制。

Objective To establish an High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry (HPLC-QQQ) method for determination of thirteen flavonoids in Ginkgo leaves preparations. Methods The separation was performed on an Agilent Poroshell 120 EC-C₁₈ (50 mm×3.0 mm, 2.7 μm) with the mobile phase consisted of 0.1% formic acid solution acetonitrile for gradient elution. The column temperature was set at 30℃, and the flow rate was 0.3 mL/min. The flavonoids were detected by electrospray ionization mass spectrometry in negative mode with multiple reaction monitoring (MRM) mode. Results Thirteen flavonoids, such as rutin, isoquercetin, quercetin-3-O-β-D-glucosyl (1→2)-α-L-rhamnoside, kaempferol-3-O-rutinoside, narcissus, quercetin, apigenin-7-O-β-D-glucopyranoside, luteolin, quercetin, apigenin, kaempferol, isorhamnetin, and genkwanin had good resolution, and showed good linear relationships in their respective mass concentration ranges (r=0.999 0). The values of RSD of precision test and repeatability test were all less than 3.5%. The sample solution was stable within 12 h. The recoveries of thirteen flavonoids were within 94.5%-100.5%. The contents of total flavonoids in Ginkgo leaves preparations from different batches had little difference, and it was quite different in different batches of samples. The proportion of flavonoid glycosides was relatively large. The contents of rutin and narcissus were higher than those of monosaccharides (isoquercitrin and quercitrin), while the contents of genkwanin and luteolin were the lowest. Conclusion The method has good separation, simple operation, and strong specificity. It can clearly reflect the distribution and difference of flavonoids in Ginkgo leaves preparations, and can be used for the quality control of Ginkgo leaves preparations.

R927.2

上海市寶山區(qū)科學技術(shù)委員會科技創(chuàng)新專項資金項目（18-E-14）