目的:建立苍术中吡咯里西啶生物碱(PAs)的含量测定方法,考察麸炒前后5个PAs的变化规律.方法:采用UPLC-MS/MS法进行含量测定,采用ACQUITY UPLCHSS T3(150mm×2.1mm,1.8μm)色谱柱,流动相为乙腈-0.1％甲酸溶液(体积比为11∶89),恒流洗脱,流速0.30 mL·min-1,进样体积1 μL;电喷雾离子源,正离子多反应监测模式,以标准曲线法计算含量.结果:3批苍术经过麸炒后,PAs总量从188.74～254.64 μg·kg-1下降到101.74～135.36 μg·kg-1;野百合碱从25.35～52.18μg·kg-1下降到23.25～37.41 μg·kg-1;氮氧化野百合碱从25.12～40.22μg·kg-1下降到6.98～18.23μg·kg-1;克氏千里光碱从 11.64～36.25 μg·kg-1下降到3.64～12.85 μg·kg-1;蓝蓟定从37.52～85.32μg·kg-1下降到32.41～38.25 μg·kg-1;氮氧化蓝蓟定从26.96～74.21 μg·kg-1下降到 11.82～26.37μg·kg-1.结论:该方法可用于苍术中PAs的测定.麸炒后PAs总量和单个含量均有降低,阐明了苍术麸炒解毒的科学内涵.

建立超高效液相色谱-串联质谱法测定木贼中4种肝毒性吡咯里西啶生物碱(石松胺、石松胺氮氧化物、蓝蓟定氮氧化物和蓝蓟定)的含量.采用ACQUITY UPLC HSS T3型色谱柱(100 mm×2.1 mm,1.8μm),以甲酸-甲酸铵缓冲液(10 mmol/L甲酸溶液-2.5 mmol/L甲酸铵溶液)-酸化乙腈(95％乙腈水溶液,含10 mmol/L甲酸溶液-2.5 mmol/L甲酸铵溶液)(体积比为85:15)为流动相,流量为0.30 mL/min,进样体积为1μL,电喷雾离子源,正离子多反应监测模式,以外标法计算含量.石松胺、石松胺氮氧化物、蓝蓟定氮氧化物和蓝蓟定在各自的质量浓度范围内与色谱峰面积线性关系良好,线性系数均不小于0.999,检测限分别为0.20、0.21、0.20、0.20 ng/mL.测定结果的相对标准偏差分别为2.5％、3.2％、3.4％、2.9％(n=6),平均加标回收率为91.9％～97.1％.该方法可为木贼中吡咯里西啶生物碱的质量控制和安全性评价提供科学依据.

目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)对马鞭草中6个肝毒性吡咯里西啶生物碱的含量进行测定,并根据测定结果进行初步的风险评估.方法:选择Waters ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以含0.05％甲酸和2.5 mmol·L-1甲酸铵的水溶液(A)及含0.05％甲酸和2.5 mmol·L-1甲酸铵的乙腈溶液(B)为流动相进行梯度洗脱(0～12 min,3％～8％B;12～25 min,8％～15％B;25～26 min,15％～3％B;26～30 min,3％B),流速0.3 mL· min-1,柱温40 ℃,进样量1μL;电喷雾离子源(ESI),正离子模式下多反应监测模式,通过优化三重四极杆的MS参数及6个分析物的MS参数进行定性、定量分析.根据含量测定结果,采用暴露限值(MOE)结合热水提取转移率进行风险评估.结果:通过仪器精密度、线性范围、重复性、稳定性和加样回收试验等方法学验证,其结果均符合定量分析的要求.印美定、石松胺、印美定氮氧化物、石松胺氮氧化物、蓝蓟定氮氧化物和蓝蓟定的线性范围分别为0.984～49.20,0.994～49.70,1.012～50.60,1.032～51.60,1.004～50.20,1.016～50.80 μg·L-1,这6个成分在线性范围内峰面积与质量浓度均具有良好线性关系(r≥0.9990);平均加样回收率在87.2％～94.2％,RSD均＜4.0％;MOE均＞1万.结论:建立的UPLC-MS/MS稳定可行,可为马鞭草中肝毒性吡咯里西啶生物碱的质量控制和安全性评价提供科学依据.

目的 采用HPLC测定云南不同产地的野生与栽培黄草乌中滇乌碱、黄草乌碱甲及黄草乌碱丙的含量.方法 采用Extend-C18色谱柱(4.6 mm×250 rnm,5μm),流动相A为乙腈、B为40 mmol/L乙酸铵缓冲液(用氨水调pH值至9.00),两相梯度洗脱(0～35 min,35％→55％A;35～40 min,55％A),流速1.0 mL/min,柱温30℃,波长260 nm.结果 7个产地野生与栽培黄草乌中滇乌碱含量为510.29～ 1837.44 μg/g,新平产野生黄草乌最高,建水栽培者最低;黄草乌碱甲含量为583.92～4105.45 μg/g,个旧栽培黄草乌(黄皮)最高,建水栽培者最低;黄草乌碱丙含量为79.93～2281.68 μg/g,嵩明产野生黄草乌最高,建水栽培者最低.3种双酯型二萜生物碱总含量为1240.32～5732.09 μg/g.HPLC对比图显示,黄草乌栽培品与野生品成分存在较大差异.结论 黄草乌野生品与栽培品存在明显成分差异,3种双酯型生物碱含量差异很大,不同产地的栽培品之间也有明显差异.

Aconitum vilmorinianum Komarov is a local medicinal plant used in many well-known clinical preparations to treat rheumatism and pains in Yunnan Province, China. Phytochemical examination of the roots of A. vilmorinianum led to the isolation of three novel imine-type norditerpenoid alkaloids named vilmorrianines E–G (1–3), and a new natural alkaloid N-desethyl-N-formyl-8-O-methyltalatisamine (4), together with 14 known alkaloids. Their structures were elucidated on the basis of spectroscopic evidence. Vilmorrianine E is the first known norditerpenoid alkaloid containing both an imine group and a three-membered ring formed by C8, C9, and C10.

Objective To conduct comparative study on the analgesic and anti-inflammatory effects as well as the acute toxicity of yunaconitine and 8-deacetyl-yunaconitine isolated from the processed products of Aconiti Knsnezoffii Radix.Methods The methods of hot plate test and writhing test were used to evaluate the analgesic effect. Anti-inflammation action was observed by the models of auricle swelling caused by dimethylbenzene. LD50 was determined by the method of Bliss.Results Yunaconitine and 8-deacetyl-yunaconitine have analgesia effect on the pain caused by hot-plate, but there were no statistically significant difference. The pain caused by acetic acid had obvious analgesic action. High and low dose of yunaconitine could significantly reduce the number of mice body torsion and extend the incubation period of pain in mice. The effect of 8-deacetyl-yunaconitine was remarkable only in the high dose. Compared with solvent group, there were little differences in inhibiting effect of auricle swelling caused by dimethylbenzene, and anti-inflammatory action was not exact. The poisonousness of yunaconitine was nearly 20 times of 8-deacetyl-yunaconitine.Conclusion Yunaconitine and 8-deacetyl-yunaconitine may be the analgesic medicine for peripheral analgesic effect. The poisonousness of 8-deacetyl-yunaconitine is less than yunaconitine, the effect is remarkable to the pain caused by acetic acid, and the security is high.