Analysis of curcuminoids and volatile components in 160 batches of turmeric samples in China by high-performance liquid chromatography and gas chromatography mass spectrometry.

Turmeric (Curcuma longa L.) is a popular herbal medicine worldwide. Curcuminoids and volatile constituents are its major bioactive components. To improve the quality control of turmeric, we determined the contents of three main curcuminoids in 160 batches of turmeric samples collected from five major production areas of China by HPLC, and analyzed the volatile components by GC/MS. The results indicated that samples with red cross sections (2.75 ±â€¯0.82 mg/g) contained significantly higher amounts of curcuminoids than samples with yellow sections (1.23 ±â€¯0.60 mg/g) (p < 0.001). This result was consistent with empirical standard of TCM pharmacists. The contents of curcuminoids in samples from Hainan (4.51±0.25%), Guizhou (3.17±0.41%), and Sichuan (2.25±0.54%) were relatively high and consistent. Moreover, the GC/MS profiles of turmeric may be affected by storage and processing. This study sets a good example for comprehensive quality control of herbal medicines.

Rapid quantitation and identification of the chemical constituents in Danhong Injection by liquid chromatography coupled with orbitrap mass spectrometry.

Danhong Injection (DHI) is a Chinese medicine patent drug to treat cardiovascular diseases. It is derived from the herbal medicines Dan-shen and Hong-hua. The bioactive compounds of DHI are polar phenolic acids and flavonoid glycosides. Thus far, the contents of major compounds in DHI are not well understood, and the identification of minor compounds lacks rapid methods. In this work, quantitative and qualitative analyses of DHI compounds were performed using ultra-high performance liquid chromatography coupled with orbitrap mass spectrometry (UHPLC/orbitrap-MS). DHI was separated on an Acquity HSS T3 column (1.8 µm, 100 mm × 2.1 mm) and eluted with acetonitrile-water (containing 0.1% formic acid) to determine the contents of 12 compounds within 6 min. The method was fully validated according to the ICH guidance. To identify the minor compounds, an ion statistics-based strategy was used to dig for 4 filtering ions and 6 diagnostic ions from 22 reference standards. A total of 117 compounds, including 76 phenolic acids, 20 flavonoids, and 21 other compounds were tentatively identified. The poor stability of salvianolic acid A upon storage was also discussed.

Simultaneous Determination and Risk Assessment of Pyrrolizidine Alkaloids in Artemisia capillaris Thunb. by UPLC-MS/MS Together with Chemometrics.

Pyrrolizidine alkaloids (PAs) are natural toxins found in some genera of the family Asteraceae. However, it has not been reported whether PAs are present in the widely used Asteraceae plant Artemisia capillaris Thunb. (A. capillaris). The purpose of this study was to establish a sensitive and rapid UPLC-MS/MS method together with chemometrics analysis for simultaneous determination and risk assessment of PAs in A. capillaris. The developed UPLC-MS/MS method was validated and was confirmed to display desirable high selectivity, precision and accuracy. Risk assessment was conducted according to the European Medicines Agency (EMA) guideline. Chemometrics analysis was performed with hierarchical clustering analysis and principal component analysis to characterize the differences between PAs of A. capillaris. Finally, PAs were found in 29 out of 30 samples and at least two were detected in each sample, besides, more than half of the samples exceeded the EMA baseline. Nevertheless, the chemometrics results suggested that the PAs contents of A. capillaris from different sources varied significantly. The method was successfully applied to the detection and risk evaluation of PAs-containing A. capillaris for the first time. This study should provide a meaningful reference for the rational and safe use of A. capillaris.

Simultaneous determination of chloramphenicol and aflatoxin M1 residues in milk by triple quadrupole liquid chromatography-tandem mass spectrometry.

A reliable, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of chloramphenicol and aflatoxin M(1) in milk has been developed. This method includes simple extraction of sample with acetonitrile, separation on a MGIII-C(18) column using 5 mM ammonium acetate aqueous solution/methanol (60:40, v/v) as mobile phase, and MS/MS detection using multiple reaction monitoring mode. The method was validated according to Commission Decision 2002/657/EC. The limits of detection (LODs) were 0.05 µg/kg for chloramphenicol and 0.005 µg/kg for aflatoxin M(1.) The limits of quantification (LOQs) were 0.2 µg/kg for chloramphenicol and 0.02 µg/kg for aflatoxin M(1). The recovery values ranged from 88.8% to 100.6%, with relative standard deviation lower than 15% in all cases, when samples were fortified at three different concentrations. The decision limits (CCα) and detection capability (CCß) of the method were also reported. This method has been successfully applied for simultaneous analysis of chloramphenicol and aflatoxin M(1) residues in milk from local supermarkets in China.

[Studies on the chemical constituents from Inula cappa (II)].

OBJECTIVE: To study the chemical constituents of the root of Inula cappa. METHOD: The compounds were isolated and purified by recrystallization and chromatography with silica gel column and Sephadex LH-20 column. Their structures were identified by physico-chemical properties and spectral analysis. RESULTS: Seven compounds were isolated as scopolin (I), octacosanoic acid (II), tritriacontane (III), (2S,3S,4R,8E)-2-[(2'R)-2'-hydroxydocosanosylamino]-octadecane-1,3,4-triol(IV),(2S,3S,4R,8E)-2-[(2'R)-2'-hydroxytricosanosylamino]-octadecane-1,3,4-triol(V), (2S,3S,4R,8E)-2-[(2'R)-2'-hydroxytetracosanosylamino]-octadecane-1,3,4-triol(VI), (2S,3S,4R,8E)-2-[(2'R)-2'-hydroxypentacosanosylamino]-octadecane-1,3,4-triol(VIII), (2S,3S,4R,8E)-2-[(2'R)-2'-hydroxyhexacosanosylamino]-octadecane-1,3,4-triol(VIII). CONCLUSION: All compounds were isolated from Inula cappa for the first time.

[Studies on chemical constituents in fruit of Rubus chingii].

OBJECTIVE: To study the chemical constituents of the fruit of Rubus chingii. METHOD: The compounds were isolated and purified by recrystallization and chromatography with silica gel column and Sephadex LH-20 column. Their structures were identified by physicochemical properties and spectral analysis. RESULT: Eleven compounds were isolated as oleanic acid (I), ursolic acid (II), maslinic acid (III), 2alpha-hydroxyursolic acid (IV), arjunic acid (V), hexacosyl p-coumarate (VI), tiliroside (VII), stearic acid (VIII), lacceroic acid (IX), beta-sitosterol (X), daucosterol (XI). CONCLUSION: Compounds I, II, III, IV, V, VI, VIII, IX, XI were isolated from R. chingii for the first time.