Rapid determination of 54 dye components in hair dyes by liquid chromatography coupled to quadrupole orbitrap high-resolution mass spectrometry.

Chemical hair dye components can have allergenic, reproductive, and carcinogenic risks. Detecting restricted and prohibited ingredients in these products is challenging due to product diversity, isomer separation, instability, and wide polarity range. A method was developed using HPLC-high-resolution mass spectrometry for the qualitative and quantitative analysis of 54 hair dye components in various products. Samples were extracted with a 70% methanol solution, ultrasonicated in an ice bath, centrifuged, filtered, diluted with 25% methanol solution and 25% methanol solution containing 0.05% D-isoascorbic acid. Separation was achieved using an ACE Excel 3 C18 column (2.1 mm × 150 mm, 3 µm) with analysis conducted via quadrupole Orbitrap mass spectrometry. It showed good linear correlations, with detection limits of 0.1-23.5 ng mL-1, and quantitation limits of 0.2-78.1 ng mL-1. Average recovery ranged from 60.0% to 118.4%, with repeatability from 4.0% to 14.9%. Stability was confirmed within 48 hours. When applied to 20 batches of commercially available hair dyes, 24 hair dye components were found within permissible levels. The method is crucial for quality control of hair dyes, covering 10 common prohibited and 44 permissible hair dye components outlined in the Safety and Technical Standards for Cosmetics (2015 Edition). Compared to the standard methods, it can separate isomers in a single mobile phase system within 15 minutes in positive ion mode while maintaining sensitivity for phenol, hydroquinone, and other components in negative ion mode. Moreover, the pre-treatment strategy significantly improved stability and accuracy, enabling precise analysis of the 54 hair dye components.

The residues and health risk assessment of polychlorinated biphenyls (PCBs) in Pheretima (an earthworm-derived traditional medicine) from southeastern China.

Minimal research exists on polychlorinated biphenyl (PCB) exposure from traditional Chinese medicines (TCMs), despite their significant contributions to domestic and international health protection. This study is the first to investigate the levels, profiles, and health risks of PCB residue in Pheretima, a typical TCM produced from earthworm. Seventy-seven Pheretima samples from different regions of China were analyzed for 45 PCB congeners. PCBs were found in all samples exhibiting species-dependent discrepancies. ∑45PCBs was ranging from 0.532 to 25.2 µg/kg (mean 4.46 µg/kg), with CB-11 being the most abundant congener contributing 71.8% ± 10.8% to ∑45PCBs, followed by CB-47, which were all non-Aroclor congeners called unintentionally produced PCBs (UP-PCBs). The average estimated daily intake of ∑45PCBs, ∑7ID-PCBs (indicative polychlorinated biphenyls), and CB-11 were 0.71, 0.04, and 0.51 ng/kg bw/d, respectively. The ∑HQ of PCBs in Pheretima samples was 2.97 × 10-4-2.46 × 10-2 (mean 2.77 × 10-3, 95th 4.21 × 10-3), while the ∑RQ ranged from 1.19 × 10-8 to 2.88 × 10-6 (mean 4.87 × 10-7, 95th 2.31 × 10-6). These findings indicate that Pheretima ingestion does not pose significant non-carcinogenic risks. However, certain individual samples exhibit an acceptable level of potential risks, particularly when considering that PCBs are recognized as endocrine disruptors and classified as probable carcinogens. These results contribute to the safety evaluation of traditional medicines and suggest the potential use of Pheretima as a bioindicator for PCB pollution. It is advisable to monitor UP-PCBs as indicator congeners and gather additional toxicological data.

Alisol B 23-acetate adjusts bile acid metabolisim via hepatic FXR-BSEP signaling activation to alleviate atherosclerosis.

BACKGROUND: Postmenopausal women have a high incidence of atherosclerosis. Phytosterols have been shown to have cholesterol-lowering properties. Alisa B 23-acetate (AB23A) is a biologically active plant sterol isolated from Chinese herbal medicine Alisma. However, the atherosclerosis effect of AB23A after menopause and its possible mechanism have not been reported yet. PURPOSE: To explore whether AB23A can prevent atherosclerosis by regulating farnesoid X receptor and subsequently increasing fecal bile acid and cholesterol excretion to reduce plasma cholesterol levels. METHODS: Aortic samples from premenopausal and postmenopausal women with ascending aortic arteriosclerosis were analyzed, and bilateral ovariectomized (OVX) female LDLR-/- mice and free fatty acid (FFA)-treated L02 cells were used to analyze the effect of AB23A supplementation therapy. RESULTS: AB23A increased fecal cholesterol and bile acids (BAs) excretion dependent on activation of hepatic farnesoid X receptor (FXR) in ovariectomized mice. AB23A inhibited hepatic cholesterol 7α-hydroxylase (CYP7A1) and sterol 12α-hydroxylase (CYP8B1) via inducing small heterodimer partner (SHP) expression. On the other hand, AB23A increased the level of hepatic chenodeoxycholic acid (CDCA), and activated the hepatic BSEP signaling. The activation of hepatic FXR-BSEP signaling by AB23A in ovariectomized mice was accompanied by the reduction of liver cholesterol, hepatic lipolysis, and bile acids efflux, and reduced the damage of atherosclerosis. In vitro, AB23A fixed abnormal lipid metabolism in L02 cells and increased the expression of FXR, BSEP and SHP. Moreover, the inhibition and silencing of FXR canceled the regulation of BSEP by AB23A in L02 cells. CONCLUSION: Our results shed light into the mechanisms behind the cholesterol-lowering of AB23A, and increasing FXR-BSEP signaling by AB23A may be a potential postmenopausal atherosclerosis therapy.

[Simultaneous determination of three kinds of components in sanhuang tablets by high-performance liquid chromatography].

AIM: To establish an assay method for the determination of three kinds of biologically active components, five compounds (emodin, chrysophanol, baicalin, wogonin and berberine hydrochloride) simultaneously in Sanhuang tablets. METHODS: HPLC was carried out, using a C18 column (150 mm x4. 6 mm ID, 5 microm) set at 30 degrees C, acetonitrile-0.02 mol x L(-1) acetic ammonium (adjusted pH to 3. 50 with acetic acid glacial) as mobile phase (using gradient) with flowing rate 1. 00 mL x min(-1) and detected at 270 nm. RESULTS: The calibration curve of emodin was linear from 0.020 7 microg to 0.207 microg with r = 0.999 9, the average recovery was 99.65% with RSD 1.25%. The calibration curve of chrysophanol was linear from 0.052 microg to 0.52 microg with r = 0.999 9, and the average recovery was 100.36% with RSD 0.96%. The calibration curve of baicalin was linear from 0.250 5 microg to 2.505 microg with r =0.999 8, and the average recovery was 100.22% with RSD 1.29%. The calibration curve of wogonin was linear from 0.047 6 microg to 0.476 microg with r = 0.999 9, and the average recovery was 98.97% with RSD 1.20%. The calibration curve of berberine hydrochloride was linear from 0.053 12 microg to 0.531 2 microg with r = 0.999 5, and the average recovery was 96.02% with RSD 2.02%. The established method had also been used in the determination of the 5 compounds in 10 different batches of Sanhuang tablets. CONCLUSION: This method was proved to be accurate and quick, and can be used for the quality control of the preparation all-around.