色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
3期
216-223
,共8页
超高效液相色谱-串联质谱%有效成分%复方杏香兔耳风胶囊
超高效液相色譜-串聯質譜%有效成分%複方杏香兔耳風膠囊
초고효액상색보-천련질보%유효성분%복방행향토이풍효낭
ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS /MS)%effective components%Fufangxingxiangtu’erfeng capsules
建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III 和白术内酯 I 等10种有效成分含量的超高效液相色谱-串联质谱（ UPLC-MS / MS）双内标分析方法。以咖啡酸和淫羊藿苷为内标（IS），在 ZORBAX RRHD Eclipse Plus C 18色谱柱上，以甲醇和含0.3％甲酸的水为流动相进行梯度洗脱分离，流速为0.3 mL / min。在电喷雾电离（ESI）正、负离子切换模式下，采用多重反应监测模式进行检测。结果表明，原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III、白术内酯 I 的线性范围分别为0.00300~24.0 mg / L、0.0170~2.00 mg / L、0.0150~30.0 mg / L、0.00400~30.0 mg / L、0.0105~24.0 mg / L、0.00300~30.0 mg / L、0.00300~5.00 mg / L、0.00600~5.00 mg / L、0.00150~4.00 mg / L、0.000600~0.900 mg / L；检出限分别为1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg / L。10种成分的加样回收率为92.5％~106％，相对标准偏差均不大于3.2％。该方法快速简便、灵敏度高、重复性好，已成功用于实际样品的分析。
建立瞭同時測定複方杏香兔耳風膠囊中原兒茶痠、原兒茶醛、綠原痠、野黃芩苷、異綠原痠 C、黃芩苷、木犀草素、芹菜素、白術內酯 III 和白術內酯 I 等10種有效成分含量的超高效液相色譜-串聯質譜（ UPLC-MS / MS）雙內標分析方法。以咖啡痠和淫羊藿苷為內標（IS），在 ZORBAX RRHD Eclipse Plus C 18色譜柱上，以甲醇和含0.3％甲痠的水為流動相進行梯度洗脫分離，流速為0.3 mL / min。在電噴霧電離（ESI）正、負離子切換模式下，採用多重反應鑑測模式進行檢測。結果錶明，原兒茶痠、原兒茶醛、綠原痠、野黃芩苷、異綠原痠 C、黃芩苷、木犀草素、芹菜素、白術內酯 III、白術內酯 I 的線性範圍分彆為0.00300~24.0 mg / L、0.0170~2.00 mg / L、0.0150~30.0 mg / L、0.00400~30.0 mg / L、0.0105~24.0 mg / L、0.00300~30.0 mg / L、0.00300~5.00 mg / L、0.00600~5.00 mg / L、0.00150~4.00 mg / L、0.000600~0.900 mg / L；檢齣限分彆為1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg / L。10種成分的加樣迴收率為92.5％~106％，相對標準偏差均不大于3.2％。該方法快速簡便、靈敏度高、重複性好，已成功用于實際樣品的分析。
건립료동시측정복방행향토이풍효낭중원인다산、원인다철、록원산、야황금감、이록원산 C、황금감、목서초소、근채소、백술내지 III 화백술내지 I 등10충유효성분함량적초고효액상색보-천련질보（ UPLC-MS / MS）쌍내표분석방법。이가배산화음양곽감위내표（IS），재 ZORBAX RRHD Eclipse Plus C 18색보주상，이갑순화함0.3％갑산적수위류동상진행제도세탈분리，류속위0.3 mL / min。재전분무전리（ESI）정、부리자절환모식하，채용다중반응감측모식진행검측。결과표명，원인다산、원인다철、록원산、야황금감、이록원산 C、황금감、목서초소、근채소、백술내지 III、백술내지 I 적선성범위분별위0.00300~24.0 mg / L、0.0170~2.00 mg / L、0.0150~30.0 mg / L、0.00400~30.0 mg / L、0.0105~24.0 mg / L、0.00300~30.0 mg / L、0.00300~5.00 mg / L、0.00600~5.00 mg / L、0.00150~4.00 mg / L、0.000600~0.900 mg / L；검출한분별위1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg / L。10충성분적가양회수솔위92.5％~106％，상대표준편차균불대우3.2％。해방법쾌속간편、령민도고、중복성호，이성공용우실제양품적분석。
Using caffeic acid and icariin as internal standards,a method for the simultaneous determination of protocatechuic acid,protocatechuic aldehyde,chlorogenic acid,scutellarin, isochlorogenic acid C,baicalin,luteolin,apigenin,atractylenolide III and atractylenolide I in Fufangxingxiangtu’erfeng capsules were established by ultra performance liquid chromatogra-phy with tandem mass spectrometry(UPLC-MS / MS). The separation was performed on a ZOR-BAX RRHD Eclipse Plus C 18 column( 50 mm × 2. 1 mm,1. 8 μm)by using water containing 0. 3% formic acid and methanol as mobile phases with the gradient elution at a flow rate of 0. 3 mL / min. The analytes were detected by a tandem mass spectrometer in the multiple reaction monitoring(MRM)mode via the switching of positive electrospray ionization(ESI +)and nega-tive electrospray ionization(ESI -). Under optimum conditions,the calibration curves were lin-ear in the range of 0. 003 00-24. 0 mg / L for protocatechuic acid,0. 017 0-2. 00 mg / L for proto-catechuic aldehyde,0. 015 0-30. 0 mg / L for chlorogenic acid,0. 004 00-30. 0 mg / L for scutella-rin,0. 010 5-24. 0 mg / L for isochlorogenic acid C,0. 003 00-30. 0 mg / L for baicalin,0. 003 00-5. 0 mg / L for luteolin,0. 006 00-1. 50 mg / L for apigenin,0. 001 50-4. 00 mg / L for atractylenol-ide III,and 0. 000 600 - 0. 900 mg / L for atractylenolide I with the detection limits of 1. 0,11, 5. 0,1. 5,3. 5,1. 0,1. 0,2. 0,0. 50,0. 20 μg / L,respectively. The average recoveries of the ten effective components were between 92. 5% and 106% with all relative standard deviations not more than 3. 2% . The developed method was rapid,simple,accurate,reproducible,and suit-able for the quality control of the Fufangxingxiangtu’erfeng capsules.
