ABSTRACT
OBJECTIVE：To optim ize ethanol extraction technology of Mongolian medicine Naru- 3. METHODS ：The L 9（34） orthogonal design was used to optimize ethanol extraction technology of Mongolian medicine Naru- 3 with solid-liquid ratio ，ethanol volume fraction and extraction time as factors ，using comprehensive scores for the contents of benzoylaconitine ，benzoylneoaconitine， benzoylhypoaconitine，aconitine，neoaconitine，hypoaconitine，piperine and gallic acid as indexes. RESULTS ：The optimal ethanol extraction technology was that solid-liquid ratio of 1∶10（g/mL），ethanol volume fraction of 75％，extracting for 1.5 h. After 3 times of validation tests ，average contents of above 8 components in ethanol extract from Naru- 3 were 1.69，1.48，14.69，0.28， 0.05，0.08，26.01，17.33 mg/g（RSDs were 0-4.96％，n＝3），respectively. Average comprehensive score was 19.03（RSD＝1.42％， n＝3）. CONCLUSIONS ：The optimal ethanol extraction technology of Mongolian medicine Naru- 3 is stable and feasible.
ABSTRACT
Objective:To establish a method for rapid determination of iodine in whole blood by direct alkali dilution inductively coupled plasma mass spectrometry (ICP-MS).Methods:Totally 0.50 ml whole blood sample was collected, and 2% ammonia and 0.01% Triton X-100 solution were added to constitute a total volume of 10.0 ml. After shaking to uniformity, 1.0 μg/ml rhodium and 20% isopropanol were used as on-line internal standard solution. The flow ratio of internal standard solution to the solution to be measured was 1∶16. The sample was quantitatively determined by ICP-MS. The linear range, limit of detection (LOD), accuracy and precision of the method were evaluated.Results:Iodine in whole blood could be determined and had a good linear relationship within the range of 0-200 μg/L, with correlation coefficient ( r) > 0.999. The LOD of the method was 0.1 μg/L, the limit of quantitation (LOQ) was 0.3 μg/L, the recovery rate of iodine in whole blood was 88.5%-106.1%, and the relative standard deviation was 2.2%-4.7% ( n=7). Conclusions:A method for rapid determination of iodine in whole blood by direct alkali dilution ICP-MS is successfully established. This method is accurate, simple, rapid, and highly automatic, and it can be widely applied in determination of iodine in whole blood.
ABSTRACT
OBJECTIVE： To establish a method for simultaneously determining the contents of 6 volatile components such as eugenol， methyl eugenol， isoeugenol， α-asarone， alkaloid and myristyl ether in Zhachong shisan. METHODS：Volatile oil was extracted by steam distillation and analyzed by gas chromatography. The chromatographic column was ov-1701， with hydrogen flame ionization detector. The carrier gas was nitrogen， the inlet temperature was 220 ℃， the detector temperature was 240 ℃， the flow rate was 1.0 mL/min， the injection volume was 1 μL， the split ratio was 10 ∶ 1， with programmed temperature. RESULTS： The linear ranges of eugenol， methyl eugenol， isoeugenol， α-asarone， costunolide and myristyl were 2.00-12.00， 1.00-6.00， 0.60-3.60， 0.05-0.30， 0.05-0.30， 0.60-3.60 mg/mL（r＝0.999 9）. The detection limits were 0.01， 0.01， 0.02， 0.01， 0.01， 0.01 mg/mL， respectively； the limits of quantification were 0.05， 0.03， 0.06， 0.02， 0.02， 0.03 mg/mL， respectively. RSDs of precision， stability and reproducible tests were all lower than 3％； average recovery rates were 99.33％-100.04％， RSDs were 0.02％-0.35％ （n＝6）； RSDs of durability test were all lower than 5％. CONCLUSIONS： The established method was simple and reproducible. It can be used for simultaneous determination of the contents of 6 volatile components in Zhachong shisan.
ABSTRACT
OBJECTIVE:To establish HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry for rapid determination of aconitine,mesaconitine,hypaconitine,benzoylaconitine,benzoylmesaconine and benzoylhypacoitine in rat plasma. METHODS:Internal standard lappaconitine was added into plasma sample,and methanol precipitated protein was used for pretreatment. HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry was adopted. HPLC condition was as follows as Sinochrom ODS-BP C18column,mobile phase consisted of acetonitrile-1% formic acid solution(50:50,V/V),the flow rate of 0.6 mL/min,sample size of 10 μL,column temperature of 25 ℃,automatic sampler temperature of 4 ℃. Mass spectrum scanning mode was full ion monitoring model,positive ion acquisition,mass charge ratios(m/z)of ion were 646.32(aconitine), 632.30(mesaconitine),616.31(hypaconitine),604.31(benzoylaconitine),590.29(benzoylmesaconine),574.30(benzoylhypacoitine), 585.31(internal standard). Six male Wistar rats were collected and given single dose of total alkaloid extract of Aconitum carmichaeli(4 mg/kg)intragastrically. Blood samples were collected before medication(0 h)and 0.5,0.75,1.25,1.5,2,4,6, 8,10,24 h after medication. Plasma concentration was determined and pharmacokinetic parameters were calculated by using PK-Solver V2.0 software. RESULTS:The linear range of 6 kinds of aconitum alkaloids in plasma were 0.1-10 μ g/L(r>0.992). The limit of quantitation was 0.1 μ g/L. Average recovery was higher than 75%,RSDs of intra-day and inter-day,matrix effects,stability test were all lower than 15%. The tmaxof 6 kinds of aconite alkaloids were about 1.2 h;t1/2were about 10 h;cmaxof monoestertype aconite alkaloids were higher than those of diester-type aconite alkaloids. CONCLUSIONS:Established HPLC-quadrupole/electrostatic field orbitrap high resolution mass spectrometry is accurate,sensitive,simple and rapid, and can be used for plasma concentration monitoring of 6 kinds of aconitum alkaloids.