超高效液相色谱-串联质谱法快速测定酒中的次乌头碱、乌头碱、中乌头碱
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摘要
建立了酒中次乌头碱、乌头碱、中乌头碱的超高效液相色谱-串联质谱测定方法,并用于市售药酒的测定。样品预处理后,采用ACQUITY UPLC BEH SHIELD RP18柱(2.1×50 mm,1.7μm)进行分离,乙腈:10 mmol/L乙酸铵水溶液(氨水调节pH9.5)为流动相进行洗脱,电喷雾离子源正离子模式下检测,测得次乌头碱、乌头碱及中乌头碱在0～5 000μg/L范围内,与峰面积呈良好线性关系,相关系数r≥0.999,相对标准偏差为0.55%～3.50%;次乌头碱、乌头碱及中乌头碱的检出限均小于0.1μg/L,定量限均小于0.3μg/L;加标水平为1μg/L、10μg/L、50μg/L时回收率为94%～100%。该方法准确可靠,简便快速,可用于药酒中次乌头碱、乌头碱、中乌头碱的测定。
An ultra performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for the determination of hypaconitine, aconitine and mesaconine in wine is established and used for the determination of commercially available medicinal liquor. After pretreatment of the sample, it was separated by ACQUITY UPLC BEH SHIELD RP18 column(2.1 mm ×50 mm, 1.7 μm), and the mobile phase is eluted with acetonitrile:10 mmol/L ammonium acetate aqueous solution(ammonia water adjusted pH 9.5). In the positive ion mode of spray ion source, the hypaconitine, aconitine and mesaconine are measured in the range of 0—5 000 μg/L, which shows a good linear relationship with the peak area. The correlation coefficient is r≥0.999, relative standard deviation is between 0.55% to 3.50%; the detection limits of hypaconitine, aconitine and mesaconine are less than 0.1 μg/L, the limit of quantification is less than 0.3 μg/L; the spiked level is 1 μg/L, and the recovery rate is between 94% to 100% at 1 μg/L, 5μg/L and 10 μg/L. The method is accurate, reliable, simple and rapid, and can be used for the determination of secondary aconitine, hypaconitine and mesaconine in medicated wine.
An ultra performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) method for the determination of hypaconitine, aconitine and mesaconine in wine is established and used for the determination of commercially available medicinal liquor. After pretreatment of the sample, it was separated by ACQUITY UPLC BEH SHIELD RP18 column(2.1 mm ×50 mm, 1.7 μm), and the mobile phase is eluted with acetonitrile:10 mmol/L ammonium acetate aqueous solution(ammonia water adjusted pH 9.5). In the positive ion mode of spray ion source, the hypaconitine, aconitine and mesaconine are measured in the range of 0—5 000 μg/L, which shows a good linear relationship with the peak area. The correlation coefficient is r≥0.999, relative standard deviation is between 0.55% to 3.50%; the detection limits of hypaconitine, aconitine and mesaconine are less than 0.1 μg/L, the limit of quantification is less than 0.3 μg/L; the spiked level is 1 μg/L, and the recovery rate is between 94% to 100% at 1 μg/L, 5μg/L and 10 μg/L. The method is accurate, reliable, simple and rapid, and can be used for the determination of secondary aconitine, hypaconitine and mesaconine in medicated wine.
引文
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[20]马芳,赵东,吴晓霞,等.LC-MS-MS法检测附子水提液中新乌头碱、次乌头碱的含量[J].中国实验方剂学杂志,2011,17(13):95-97.
[2]白向阳.川乌的毒性与抗肿瘤作用概述[J].实用中医药杂志,2005,21(2):125-126.
[3]李福全,李志勇,王朝鲁,等.蒙药草乌毒性研究进展[J].中国民族医药杂志,2011(3):65-67.
[4]邢跃文.川乌炮制和毒性的关系[J].中国民间疗法,2004,12(3):43-44.
[5]汤春红,肖雷,段海真,等.乌头碱致中枢神经毒性机制的研究进展[J].广西医学,2018,40(20):2448-2451.
[6]李荣,马立如.自制川乌草乌药酒致3例急性药物中毒病例分析[J].中国实用医药,2008,3(20):119-120.
[7]李君,张微,赛那,等.紫外-可见分光光度法测定那如-3药材提取物中乌头碱含量[J].北方药学,2018,15(12):1-2.
[8]柴宜民,刘俊芳,刘二保,等.光度法测定尿液中乌头碱的含量[J].山西师范大学学报:自然科学版,2005,19(4):57-59.
[9]曹志红,赵远.四逆汤中总乌头碱含量的测定[J].中国中医急症,2003,12(6):559.
[10]曹晖.香港市售乌头类药材及其炮制品的乌头碱含量测定[J].中国中药杂志,1993,18(5):279-281.
[11]彭蔚,肖学成,袁晓.薄层色谱法检测药酒中乌头碱[J].实用预防医学,2004,11(6):1283-1284.
[12]尉志文,刘洁,贠克明,等.薄层色谱扫描法快速检测乌头碱中毒[J].中国卫生检验杂志,2008,18(9):1746-1747.
[13]杨工昶.双波长薄层扫描法测定四知堂药酒中乌头碱含量[J].时珍国医国药,2001,12(3):218-219.
[14]昝珂,旺杰次仁,鲁静,等.HPLC测定蒙药材草乌叶中4种双酯型二萜生物碱含量[J].中国中药杂志,2018,43(4):766-771.
[15]李红海,余陆生,金鸣.高效液相色谱法分离测定药酒中乌头碱的含量[J].法医学杂志,2005,21(1):34-35.
[16]张剑,李珺沫,蒋晔.小活络丸中痕量毒性成分乌头碱的快速限量检测[J].中成药,2009,31(10):1543-1546.
[17]李娅萍,聂晶,田颂九,等.毛细管电泳柱头场强富集技术测定康复新胶囊中3种双酯型乌头碱含量[J].药物分析杂志,2004(1):37-40.
[18]超高效液相色谱-质谱联用法测定藏药萨热十三味鹏鸟丸中乌头碱类含量[J].中国药业,2016,25(18):25-29.
[19]张园,陈波,张美玲,等.超高效液相色谱-质谱联用法测定生物检材中乌头碱[J].中国法医学杂志,2018,33(1):68-70.
[20]马芳,赵东,吴晓霞,等.LC-MS-MS法检测附子水提液中新乌头碱、次乌头碱的含量[J].中国实验方剂学杂志,2011,17(13):95-97.