Ultra-rapid determination of andrographolide and dehydroandrographolide in Andrographis Herba by solid phase extraction and liquid chromatography with mass spectrometry

IF 1.7 4区 化学 Q3 CHEMISTRY, ANALYTICAL
Zhengming Qian, J. Chen, Qing-Qing Lei, Da Li, Guoying Tan, Juying Xie, Wenqing Li
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引用次数: 0

Abstract

An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (30 × 2.1 mm, 2.7 μm) and eluted with 0.5 mmol L−1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min−1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD = 2.2%) and 97.7% (RSD = 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultra-rapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.
固相萃取-液相色谱-质谱法超快速测定穿心莲中穿心莲内酯和脱水穿心莲苷
采用液相色谱-质谱联用技术建立了穿心莲中穿心莲内酯和脱水穿心莲苷的超快速分析方法。用10 mL 40%(v/v)甲醇,然后用C18固相萃取柱纯化。LC分离在Poroshell 120上进行 EC-C18柱(30 × 2.1 毫米,2.7 μm),用0.5洗脱 mmol L−1乙酸铵水溶液和乙腈(65:35),流速为0.7 mL min−1,并通过质谱法(MS)进行检测。LC-MS分析时间小于1 min.新方法具有良好的线性(r>0.9900)、精密度和重复性(RSD<2.0%),穿心莲内酯和脱氢穿心莲苷的回收率分别为93.5%(RSD=2.2%)和97.7%(RSD=2.4%)。该方法已成功应用于7批AH样品中穿心莲内酯和脱水穿心莲固体的测定,所有样品中分析物的含量均符合中国药典的相关验收标准(>0.8%),这将有助于提高AH样本测试的效率和降低成本。
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来源期刊
Acta Chromatographica
Acta Chromatographica 化学-分析化学
CiteScore
4.00
自引率
0.00%
发文量
55
审稿时长
2.3 months
期刊介绍: Acta Chromatographica Open Access Acta Chromatographica publishes peer-reviewed scientific articles on every field of chromatography, including theory of chromatography; progress in synthesis and characterization of new stationary phases; chromatography of organic, inorganic and complex compounds; enantioseparation and chromatography of chiral compounds; applications of chromatography in biology, pharmacy, medicine, and food analysis; environmental applications of chromatography; analytical and physico-chemical aspects of sample preparation for chromatography; hyphenated and combined techniques; chemometrics and its applications in separation science.
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