高效液相色譜—質譜法同時測定辛夷提取物中4種木脂素成分

趙鑫等

摘 要 建立了高效液相色譜質譜電霧式檢測器（HPLCMSCAD）聯(lián)用技術同時測定辛夷中4種木脂素類成分的定量分析方法。采用YMCPack ODSA（250 mm×4.6 mm， 5 μm）色譜柱，甲醇水梯度洗脫，柱溫25 ℃， 流速1 mL/min，檢測波長278 nm，紫外檢測器后3∶7分流，分別進入質譜和電霧式檢測器進行檢測。以木蘭脂素為內參物，建立松脂素二甲醚、里立脂素B二甲醚和表木蘭脂素A與內參物的相對校正因子，并進行含量計算，實現(xiàn)一測多評。同時采用外標法測定辛夷提取物中4種木脂素成分的含量，比較計算值與實測值的差異，驗證所建立方法的準確定。

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Simultaneous Determination of Four Lignans in Magnoliae Flos

Extract by High Performance Liquid Chromatography

Electrospray Ionization Mass Spectrometry

ZHAO Xin1， YANG Guang2，3， ZHENG GuoShuai2，3， HANG TaiJun*1， FAN GuoRong*2，3

1（School of Pharmacy， China Pharmaceutical University， Nanjin 210009， China）

2（School of Pharmacy， Second Military Medical University， Shanghai 200433， China）

3（Shanghai Key Laboratory for Pharmaceutical （Chinese Materia Medica） Metabolite Research， Shanghai 200433， China）

Abstract A high performance liquid chromatographyelectrospray ionization mass spectrometry charged aerosol detection （HPLCMSCAD） method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMCPack ODSA column （250 mm× 4.6 mm， 5 μm） by gradient elution with methanol and water as the mobile phase at aflow rate of 1.0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0.3 mL/min and CAD detector at a flow rate of 0.7 mL/min by a split ratio of 3∶7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muticomponents by single maker （QAMS） to determine pinoresinol dimethylether， magnoli， 1irioresinol B dimethylethe and epi magnoli A . Magnoli was selected as internal standard and the relative correction factors （RCF） of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition， the limits of detection of pinoresinol dimethylether， magnoli， lirioresinol B dimethylethe and epimagnoli A were 0.34， 0.55， 0.50 and 0.58 mg/L， respectively， while the linear range were within 6.8-270 mg/L， 11-546 mg/L， 2.0-101 mg/L and 2.3-116 mg/L. The recoveries （n=9） were 98.2%-99.5%， and the correlation coefficient were 0.9995-0.9998. No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate， feasible， and can be used for quality evaluation of Magnoliae Flos .

Keywords Magnoliae Flos ； High performance liquid chromatography； Mass spectrometry； Charged aerosol detector； Lignans

（Received 1 September 2014； accepted 11 October 2014）

This work was supported by the National Natural Science Foundation of China （No.81173019）

2（School of Pharmacy， Second Military Medical University， Shanghai 200433， China）

3（Shanghai Key Laboratory for Pharmaceutical （Chinese Materia Medica） Metabolite Research， Shanghai 200433， China）

Abstract A high performance liquid chromatographyelectrospray ionization mass spectrometry charged aerosol detection （HPLCMSCAD） method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMCPack ODSA column （250 mm× 4.6 mm， 5 μm） by gradient elution with methanol and water as the mobile phase at aflow rate of 1.0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0.3 mL/min and CAD detector at a flow rate of 0.7 mL/min by a split ratio of 3∶7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muticomponents by single maker （QAMS） to determine pinoresinol dimethylether， magnoli， 1irioresinol B dimethylethe and epi magnoli A . Magnoli was selected as internal standard and the relative correction factors （RCF） of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition， the limits of detection of pinoresinol dimethylether， magnoli， lirioresinol B dimethylethe and epimagnoli A were 0.34， 0.55， 0.50 and 0.58 mg/L， respectively， while the linear range were within 6.8-270 mg/L， 11-546 mg/L， 2.0-101 mg/L and 2.3-116 mg/L. The recoveries （n=9） were 98.2%-99.5%， and the correlation coefficient were 0.9995-0.9998. No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate， feasible， and can be used for quality evaluation of Magnoliae Flos .

Keywords Magnoliae Flos ； High performance liquid chromatography； Mass spectrometry； Charged aerosol detector； Lignans

（Received 1 September 2014； accepted 11 October 2014）

This work was supported by the National Natural Science Foundation of China （No.81173019）

2（School of Pharmacy， Second Military Medical University， Shanghai 200433， China）

3（Shanghai Key Laboratory for Pharmaceutical （Chinese Materia Medica） Metabolite Research， Shanghai 200433， China）

Abstract A high performance liquid chromatographyelectrospray ionization mass spectrometry charged aerosol detection （HPLCMSCAD） method was established for the simultaneous quantitative analysis of four Lignans in Magnoliae Flos extract. The components were separated on a YMCPack ODSA column （250 mm× 4.6 mm， 5 μm） by gradient elution with methanol and water as the mobile phase at aflow rate of 1.0 mL/min. Then the elution solution was routed into MS equipment at a flow rate of 0.3 mL/min and CAD detector at a flow rate of 0.7 mL/min by a split ratio of 3∶7 for the further detection. The column temperature was 25 ℃ and the detection wavelength was 278 nm. A method was developed for the quantitative analysis of muticomponents by single maker （QAMS） to determine pinoresinol dimethylether， magnoli， 1irioresinol B dimethylethe and epi magnoli A . Magnoli was selected as internal standard and the relative correction factors （RCF） of the four Lignans were calculated. The contents of the four Lignans in Magnoliae Flos extract were determined by both external standard method and QAMS. The QAMS method was evaluated by comparison of its assay result and that of external standard method. Under the selected chromatographic condition， the limits of detection of pinoresinol dimethylether， magnoli， lirioresinol B dimethylethe and epimagnoli A were 0.34， 0.55， 0.50 and 0.58 mg/L， respectively， while the linear range were within 6.8-270 mg/L， 11-546 mg/L， 2.0-101 mg/L and 2.3-116 mg/L. The recoveries （n=9） were 98.2%-99.5%， and the correlation coefficient were 0.9995-0.9998. No significant differences were found between the quantitative results of external standard method and QAMS method. The developed method is accurate， feasible， and can be used for quality evaluation of Magnoliae Flos .

Keywords Magnoliae Flos ； High performance liquid chromatography； Mass spectrometry； Charged aerosol detector； Lignans

（Received 1 September 2014； accepted 11 October 2014）

This work was supported by the National Natural Science Foundation of China （No.81173019）