长柄扁桃加工产品中苦杏仁苷及其降解产物野黑樱苷质谱定性和定量分析
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摘要
建立了长柄扁桃加工产品中苦杏仁苷及其降解产物野黑樱苷的定性和定量分析方法。长柄扁桃饼(粕)、长柄扁桃油样品经甲醇超声萃取后,采用HPLC-Q-TOF,经C18柱(100 mm×2. 1mm,2. 7μm)分离进行定性分析;采用UPLC-TSQ,在C18柱(100 mm×2. 1 mm,1. 7μm),电喷雾ESI源,正离子模式条件下进行定量分析。结果表明:建立的定性方法,经相对保留时间、精确相对分子质量和二级碎片比对,鉴定出苦杏仁苷及其降解产物野黑樱苷;建立的定量方法对于饼粕、油脂样品中苦杏仁苷和野黑樱苷线性范围分别为50～1 000 ng/m L,50～800 ng/m L;对于饼粕样品苦杏仁苷、野黑樱苷平均加标回收率分别为99. 2%～100. 5%和102. 0%～105. 8%,精密度分别为0. 1%～3. 3%和1. 6%～3. 6%,检出限分别为2. 5、5 mg/kg;对于油脂样品苦杏仁苷、野黑樱苷平均加标回收率分别为99. 1%～108. 3%和102. 9%～108. 9%,精密度分别为1. 5%～2. 2%和1. 0%～3. 5%,检出限分别为0. 06、0. 12 mg/kg。该定量方法快速简便,为保障长柄扁桃加工产品的安全提供了技术支撑。
The method for the qualitative and quantitative analysis of amygdalin and prunasin in Amygdalus pedunculate Pall processing products was established. Amygdalus pedunculate Pall cake( meal) and Amygdalus pedunculate Pall oil were ultrasonically extracted by methanol. The qualitative analysis was performed on HPLC-Q-TOF. The sample was separated by C18 column( 100 mm × 2. 1 mm,2. 7μm). The quantitative analysis was performed on UPLC-TSQ using electrospray ionization with positive ion mode. The separation was carried out on C18 column( 100 mm × 2. 1 mm,1. 7 μm). The results indicated that based on the retention time,accurate relative molecular weight,and the product ions,the structure of amygdalin and its degradation product prunasin were determined the linear ranges of amygdalin and prunasin were 50-1 000 ng/mL for Amygdalus pedunculate Pall cake( meal) and 50-800 ng/mL for Amygdalus pedunculate Pall oil,and the average recovery rates of amygdalin and prunasin in Amygdalus pedunculate Pall cake( meal) were99. 2%-100. 5% and 102. 0%-105. 8%,with relative standard deviations of 0. 1%-3. 3% and1. 6%-3. 6%. The limits of detection for amygdalin and prunasin were 2. 5 mg/kg and 5 mg/kg,respectively. For Amygdalus pedunculate Pall oil,the average recovery rates of amygdalin and prunasin were 99. 1%-108. 3% with relative standard deviation 1. 5%-2. 2% and 102. 9%-108. 9%with relative standard deviation 1. 0%-3. 5%,and the limits of detection for amygdalin and prunasin were 0. 06 mg/kg and 0. 12 mg/kg,respectively. The method was fast and simple,which provided technical support for the safety of Amygdalus pedunculate Pall processing products.
The method for the qualitative and quantitative analysis of amygdalin and prunasin in Amygdalus pedunculate Pall processing products was established. Amygdalus pedunculate Pall cake( meal) and Amygdalus pedunculate Pall oil were ultrasonically extracted by methanol. The qualitative analysis was performed on HPLC-Q-TOF. The sample was separated by C18 column( 100 mm × 2. 1 mm,2. 7μm). The quantitative analysis was performed on UPLC-TSQ using electrospray ionization with positive ion mode. The separation was carried out on C18 column( 100 mm × 2. 1 mm,1. 7 μm). The results indicated that based on the retention time,accurate relative molecular weight,and the product ions,the structure of amygdalin and its degradation product prunasin were determined the linear ranges of amygdalin and prunasin were 50-1 000 ng/mL for Amygdalus pedunculate Pall cake( meal) and 50-800 ng/mL for Amygdalus pedunculate Pall oil,and the average recovery rates of amygdalin and prunasin in Amygdalus pedunculate Pall cake( meal) were99. 2%-100. 5% and 102. 0%-105. 8%,with relative standard deviations of 0. 1%-3. 3% and1. 6%-3. 6%. The limits of detection for amygdalin and prunasin were 2. 5 mg/kg and 5 mg/kg,respectively. For Amygdalus pedunculate Pall oil,the average recovery rates of amygdalin and prunasin were 99. 1%-108. 3% with relative standard deviation 1. 5%-2. 2% and 102. 9%-108. 9%with relative standard deviation 1. 0%-3. 5%,and the limits of detection for amygdalin and prunasin were 0. 06 mg/kg and 0. 12 mg/kg,respectively. The method was fast and simple,which provided technical support for the safety of Amygdalus pedunculate Pall processing products.
引文
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[9]高萌,王跃生,魏惠珍,等.超高效液相色谱-串联四极杆飞行时间质谱和超高效液相色谱-串联三重四极杆质谱用于血浆中苦杏仁苷及其代谢产物野黑樱苷的定性和定量分析[J].色谱,2014,32(6):591-599.
[10]LI X B,SHI F G,GU P,et al.A sensitive LC-MS/MSmethod for simultaneous determination of amygdalin and paeoniflorin in human plasma and its application[J].Pharmaceut Biomed,2014,92:160-164.
[2]邢国秀,李楠,杨美燕,等.天然苦杏仁苷的研究进展[J].中成药,2003,25(12):1007-1009.
[3]刘萍.长柄扁桃仁中苦杏仁苷及蛋白粉提取工艺研究[D].西安:西北大学,2010.
[4]吴迪,王建中,赵云霞,等.苦杏仁苷几种测定方法的比较研究[J].食品工业科技,2006(2):184-189.
[5]吴昭晖,游文玮.HPLC-ELSD法测定苦杏仁中苦杏仁苷含量的研究[J].第一军医大学学报,2005,25(12):1549-1551.
[6]钱平,贾云,刘志辉,等.高效液相色谱法测定郁李仁中苦杏仁苷的含量[J].中国中医药信息杂志,2009,16(12):50-51.
[7]中华人民共和国药典委员会.中华人民共和国药典(一部)(2010年版)[M].北京:化学工业出版社,2010:187,260.
[8]寇凯,许宁侠,申烨华.反相高效液相色谱法测定长柄扁桃仁产品中苦杏仁苷含量[J].分析科学学报,2013,29(3):367-370.
[9]高萌,王跃生,魏惠珍,等.超高效液相色谱-串联四极杆飞行时间质谱和超高效液相色谱-串联三重四极杆质谱用于血浆中苦杏仁苷及其代谢产物野黑樱苷的定性和定量分析[J].色谱,2014,32(6):591-599.
[10]LI X B,SHI F G,GU P,et al.A sensitive LC-MS/MSmethod for simultaneous determination of amygdalin and paeoniflorin in human plasma and its application[J].Pharmaceut Biomed,2014,92:160-164.