An analytical method for 10 mycotoxins in Hippophae Fructus medicinal and edible products was established in this study, and the contamination of their mycotoxins was analyzed. First of all, the mixed reference solution of ten mycotoxins such as aflatoxin, ochratoxin, zearalenone, and dexoynivalenol was selected as the control, and the Hippophae Fructus medicinal and edible products were prepared. Secondly, based on the ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) technology, 10 mycotoxins in Hippophae Fructus medicinal and edible products were quantitatively investigated and their content was determined. Finally, the contamination of mycotoxins was analyzed and evaluated. The optimal analysis conditions were determined, and the methodological inspection results showed that the 10 mycotoxins established a good linear relationship(r>0.99). The method had good repeatability, test sample specificity, stability, and instrument precision. The average recovery rates of 10 mycotoxins in Hippophae Fructus medicinal products, edible solids, and edible liquids were 90.31%-109.4%, 87.86%-107.8%, and 85.61%-109.1%, respectively. Relative standard deviation(RSD) values were 0.22%-10%, 0.75%-13%, and 0.84%-8.5%, repsectively. Based on UPLC-MS/MS technology, the simultaneous determination method for the limits of 10 mycotoxins established in this study has fast detection speed, less matrix interference, high sensitivity, and accurate results, which is suitable for the limit examination of 10 mycoto-xins in Hippophae Fructus medicinal and edible products.
Mycotoxins/analysis* ; Chromatography, Liquid/methods* ; Tandem Mass Spectrometry/methods* ; Hippophae ; Limit of Detection ; Chromatography, High Pressure Liquid/methods*

Objective: To establish a graphite furnace atomic absorption spectrometry method for the determination of trace gallium in whole blood. Methods: From January to May 2021, the five factors of ashing temperature, ashing time, atomization temperature, atomization time and matrix modifier concentration in the determination of gallium in whole blood by graphite furnace atomic absorption spectrometry were optimized by using L(16) (4(5)) orthogonal test design. At the same time, within-run, between-run, spiking recovery test and other methodological indicators were tested. Results: Under the optimized detection conditions, the linear range of determination of gallium in whole blood by graphite furnace atomic absorption spectrometry was 0.29-100.00 μg/L (r=0.9991) . The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 10.0, 50.0, 80.0 μg/L concentration levels were 2.3%-4.4% and 1.5%-3.6%, the recovery rate of spiking was 98.1%-103.8%, and the detection limit of the method was 0.13 μg/L. Conclusion: Graphite furnace atomic absorption spectrometry for the determination of trace gallium in whole blood is easy to operate, has a wide linear range, low detection limit, accurate and reliable results, which is suitable for occupational health examinations and the determination of acute gallium poisoning.
Spectrophotometry, Atomic/methods* ; Graphite/chemistry* ; Gallium ; Limit of Detection ; Temperature

OBJECTIVES: To establish a combined high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) method to detect the synthetic cannabinoid CUMYL-PEGACLONE in e-cigarette oil and hair. METHODS: HPLC-MS/MS and GC-MS were used to establish the detection method of CUMYL-PEGACLONE, and the hair of drug-involved persons and the seized e-cigarette oil were detected. RESULTS: The main mass spectrometry characteristic ions m/z of CUMYL-PEGACLONE measured by GC-MS were 91, 179, 197, 254 and 372. CUMYL-PEGACLONE had a good linear relationship in the mass concentration range of 2-50 ng/mL, and the linear correlation coefficient (r) was greater than 0.99. The limit of detection (LOD) of CUMYL-PEGACLONE in hair was 0.01 ng/mg, and the limit of quantitation (LOQ) was 0.02 ng/mg. The LOD of CUMYL-PEGACLONE in e-cigarette oil was 1 ng/mg, and the LOQ was 2 ng/mg. The average recoveries of CUMYL-PEGACLONE under the attempt at high, intermediate and low levels in blank human hair and e-cigarette oil matrix were 98.2%-132.4% and 93.5%-110.6%, and the intraday and intraday precision were 1.2%-12.9% and 0.7%-2.9%. CUMYL-PEGACLONE was detected in the hair of 15 drug-involved persons. Except for 1 person who was lower than LOQ, the concentration of CUMYL-PEGACLONE in the hair of other 14 persons was 0.035-0.563 ng/mg. The mass fraction of CUMYL-PEGACLONE in 2 e-cigarette oil were 0.17% and 0.21%, respectively. CONCLUSIONS The established HPLC-MS/MS and GC-MS methods are applied to the detection of HPLC-MS/MS in drug-related cases, which provides strong evidence support for the handling authority to quickly investigate these cases, and also provides a reference for the identification of such substances in future.
Humans ; Illicit Drugs/analysis* ; Tandem Mass Spectrometry ; Electronic Nicotine Delivery Systems ; Cannabinoids ; Hair/chemistry* ; Limit of Detection ; Substance Abuse Detection/methods*

Objective To establish a method combining QuEChERS and ultra-high liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） for rapid screening and testing of three types of new psychoactive tryptamines in human blood： 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT. Methods The effects of the type of extractant, the type and dosage of salting-out agent, and the dosage of adsorbent on the test results of the three tryptamines were investigated. Blood samples were processed by QuEChERS method and then determined by UPLC-MS/MS. Results The linear relationships of 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT in human blood were good in the range of 0.5-100, 0.5-100 and 0.2-100 ng/mL, respectively, with their coefficients higher than 0.99. The limits of detection （LODs） were 0.1-0.2 ng/mg. The recoveries ranged from 84.86% to 94.57%. Intra-day and inter-day precisions were good. Conclusion The method is simple, rapid, easy to operate and has a high recovery. It is suitable for the qualitative and quantitative study of tryptamines in blood and can provide the reference for public security organs to deal with related cases.
Chromatography, High Pressure Liquid ; Chromatography, Liquid ; Humans ; Limit of Detection ; Tandem Mass Spectrometry ; Tryptamines

Objective To establish a qualitative and quantitative method to determine ammonia in biological samples by gas chromatography-mass spectrometry （GC-MS）. Methods A heptafluorobutyryl chloride derivatization method was used. GC-MS was used for determination. The effects of different pH conditions, derivatization temperature, time and different extraction solvents on the test results were investigated. The pretreatment conditions were optimized. Results This method could accurately detect the ammonia content in blood, and the limit of detection was determined to be 0.1 μg/mL. The target component showed good linearity in the range of 0.5-200.0 μg/mL （R²=0.987 7）. The relative standard deviation range of intra-day precision was 2.59%-3.88%. The relative standard deviation range of inter-day precision was 3.21%-3.76%. Conclusion The method showed good sensitivity, stability and specificity, therefore can be used for forensic toxicology analysis and clinical biochemical detection.
Ammonia ; Gas Chromatography-Mass Spectrometry ; Limit of Detection ; Reproducibility of Results ; Solvents

Objective To establish a method for determination of escitalopram in biological samples by ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry （GC-MS/MS） and provide evidences for forensic determination of cases related to escitalopram. Methods The 1-hexyl-3-methylimidazolium hexafluorophosphate （[C₆MIM][PF₆]） was selected as an extract solvent to process biological samples. Ultrasound-assisted extraction was used on the samples. Then the samples were detected by GC-MS/MS. Results The linear range of escitalopram in blood and liver were 5.56-1 111.10 ng/mL and 0.025-5.00 mg/g, respectively. The correlation coefficient （r） were greater than 0.999, limit of detection （LOD） were 4.00 ng/mL and 2.00 μg/g, limit of quantitation （LOQ） were 14.00 ng/mL and 6.00 μg/g, respectively. The extraction recovery rates were all greater than 50%, the interday and intraday precision were less than 20%. Escitalopram was detected in blood and liver samples from the actual poisoning case by this method with a content of 1.26 μg/mL and 0.44 mg/g, respectively. Conclusion The ultrasound-assisted ionic liquid-dispersive liquid-liquid microextraction combined with GC-MS/MS is environment friendly, rapid, has good enriching effect and consumes less organic solvent and can be used for forensic determination of escitalopram related cases.
Citalopram ; Gas Chromatography-Mass Spectrometry ; Limit of Detection ; Liquid Phase Microextraction ; Tandem Mass Spectrometry

To establish a novel colloidal gold immunochromatography assay (GICA) for rapid, sensitive and accurate detection of Haemophilus influenzae infection by using the outer membrane protein P6 as detection target. First, the linear antigen epitope located in the extracellular domain of the P6 protein (GenBank accession number: AGH02799) was predicted by bioinformatics analysis. The region (62-75 aa of the protein) with strong antigen specificity was chosen and synthesized. Two rabbits were then immunized by the polypeptides (14 aa) for production of polyclonal antibodies. Then, the recombinant P6 proteins were also obtained to produce polyclonal antibodies. Finally, based on the two antibodies, a novel colloidal GICA for detection of Haemophilus influenzae infection was established and the specificity, sensitivity, repeatability and stability of this method were evaluated. At the same time, the method was tested in clinical simulation, and the plate culture method was used to verify its accuracy. The test strip for Haemophilus influenzae infection was successfully prepared. The detection limit of the test strip was as low as 1×105 CFU/mL and the whole process can be completed within 15 minutes. The strip specifically recognized Haemophilus influenzae and did not react with nine of other common respiratory pathogens such as Streptococcus pneumoniae, Moraxella catarrhalis, Mycoplasma pneumonia, and Legionella pneumophila. And the strips could be stored at 25 °C for at least 6 months without losing sensitivity or specificity. The coincidence rate between the results of 200 clinical samples and the plate culture method was 90.5%. Haemophilus influenzae protein P6, which possessed a high degree of surface antigen accessibility and antigencity, could be used as a marker for Haemophilus influenzae detection. The immunochromatographic colloidal gold test strip which bears the features of rapidity, convenience and sensitivity provides a unique tool for the on-site surveillance and diagnosis of Haemophilus influenzae infection in clinical test.
Animals ; Chromatography, Affinity ; instrumentation ; Diagnostic Tests, Routine ; standards ; Gold Colloid ; chemistry ; Haemophilus Infections ; diagnosis ; Haemophilus influenzae ; Humans ; Limit of Detection ; Rabbits ; Sensitivity and Specificity

BACKGROUND: Previous studies have reported that exposure to paraben (Pb) and triclosan (TCS) is associated with allergies. However, Pb and TCS exposure in the Japanese population is not fully understood. OBJECTIVES: The present study was aimed to examine such exposure among Japanese individuals with allergic diseases. METHODS: This cross-sectional study included the International Study of Asthma and Allergies in Childhood questionnaire survey to evaluate allergic outcomes and the collection of urine samples to examine Pb and TCS exposure. RESULTS: Pb containing daily commodities was used in 84.8% children. Pb use was positively associated with current atopic dermatitis (adjusted odds ratio, 4.61; 95% confidence interval, 1.23–17.3). Urinary Pb concentrations were increased significantly in those with current atopic dermatitis (AD) (median, 4.58 vs. 0; p < 0.0001), and showed an increased tendency in those with current wheeze (median, 3.45 vs. 1.81; p = 0.0535) in participants ≤15 years old. Urinary TCS concentration was under the limit of detection in all children. CONCLUSION: Urinary levels of Pb were associated with current AD in children. We should pay more attention about Pb and TCS.
Asian Continental Ancestry Group ; Asthma ; Child ; Cross-Sectional Studies ; Dermatitis, Atopic ; Humans ; Hypersensitivity ; Limit of Detection ; Odds Ratio ; Respiratory Sounds ; Triclosan

In this study, the marker compounds of Curcumae Rhizoma (CR) were simultaneously quantified by high-performance liquid chromatography equipped with a photodiode array detector and the anti-inflammatory effects of CR extract and marker compounds in human benign prostatic hyperplasia epithelial-1 (BPH-1) cell lines were investigated. The marker components (4S,5S)-(+)-germacrone-4,5-epoxide, furanodienone, and germacrone, were separated on Gemini C₁₈ columns (250 mm × 4.6 mm, 5 µm) at 40 ℃ by using a gradient of two mobile phases eluting at 1.0 mL/min. Prostaglandin E₂ (PGE₂) levels in Human BPH-1 cells were determined with an ELISA kit. The coefficients of determination in a calibration curve of each analyte were all 0.9997. The limits of detection and quantification of the three compounds were 0.10 – 0.32 µg/mL and 0.30 – 0.98 µg/mL, respectively. The content of three compounds, (4S,5S)-(+)-germacrone-4,5-epoxide, furanodienone, and germacrone, in the CR sample were found to be 5.79 – 5.92 mg/g, 4.72 – 4.86 mg/g, and 1.06 – 1.09 mg/g, respectively. Regarding pharmacological activity against benign prostatic hyperplasia, CR and its components significantly suppressed PGE₂ levels of BPH-1 cells. The established analysis method will help to improve quality assessment of CR samples and related products. In addition, CR and its components exhibit anti-inflammatory activity in BPH-1 cells, suggesting the inhibitory efficacy of these compounds against the pathogenesis of BPH.
Calibration ; Cell Line ; Chromatography, Liquid ; Curcuma ; Enzyme-Linked Immunosorbent Assay ; Humans ; Limit of Detection ; Methods ; Prostatic Hyperplasia ; Rhizome

BACKGROUND: 5-chloro-2-(2,4-dichlorophenoxy)phenol (triclosan) is used as an antiseptic and is a potential endocrine-disrupting chemical that can affect thyroid hormone levels. This study evaluated the relationship between triclosan exposure and thyroid hormones. METHODS: Data from the second Korean National Environmental Health Survey (2012–2014) were analyzed. Triclosan exposure was evaluated using urinary triclosan concentrations and classified into 2 groups: ‘below detection (< limit of detection [LOD])’ vs. ‘detected (≥ LOD).’ Multiple linear regression analysis was conducted to determine the relationship between triclosan exposure and the serum thyroid hormone concentrations, adjusting for age, body mass index, urinary creatinine, and smoking status. RESULTS: When grouped by sex, triclosan exposure was positively associated with the serum thyroid-stimulating hormone (TSH) concentrations in females with marginal significance (β = 0.066, p = 0.058). However, no significant association was identified between triclosan exposure and serum total triiodothyronine and thyroxine in both males and females, and TSH in males. CONCLUSIONS: This study is the first human study to evaluate the relationship between triclosan exposure and serum thyroid hormone concentrations in the Korean population. There was suggestive positive association between triclosan exposure and the serum TSH in females. Further studies need to evaluate the relationship between long-term exposure to low-dose triclosan and thyroid hormones.
Body Mass Index ; Creatinine ; Environmental Health ; Female ; Humans ; Limit of Detection ; Linear Models ; Male ; Smoke ; Smoking ; Thyroid Gland ; Thyroid Hormones ; Thyrotropin ; Thyroxine ; Triclosan ; Triiodothyronine