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*

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 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

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

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

BACKGROUND: The Automated Fluorescent Immunoassay System (AFIAS) rotavirus assay (Boditech Med Inc., Chuncheon, Korea) is a new rapid antigen test for rotavirus detection. We evaluated the performance of this assay for detecting rotaviruses and their specific genotypes in clinical stool samples. METHODS: AFIAS rotavirus assay was performed in 103 rotavirus-positive and 103 rotavirus-negative stool samples (confirmed by both PCR and ELISA), and its results were compared with those of PCR, ELISA, and immunochromatographic assay (ICA). We evaluated diagnostic sensitivity/specificity, the detectability of rotavirus subtypes, lower limit of detection (LLOD), reproducibility, cross-reactivity, and interference of AFIAS rotavirus assay. RESULTS: Based on PCR and ELISA results, diagnostic sensitivity and specificity of the AFIAS rotavirus assay were both 99.0%. LLOD results showed that the AFIAS assay had sensitivity similar to or greater than ICA and ELISA. High reproducibility was confirmed, and no cross-reactivity or interference was detected. This assay could detect genotypes G1P[8], G2P[4], G3P[8], G4P[6], G4P[8], G8P[4], G8P[8], G9P[4], and G9P[8]. CONCLUSIONS: The AFIAS rotavirus assay showed high reproducibility, sensitivity, and specificity as well as excellent agreement with ELISA, PCR, and ICA. It detected the most common as well as unusual genotypes of rotavirus prevalent in Korea. It could be a useful on-site assay for rapid, convenient, and cost-effective detection of rotavirus infection.
Enzyme-Linked Immunosorbent Assay ; Gangwon-do ; Genotype ; Immunoassay* ; Immunochromatography ; Korea ; Limit of Detection ; Polymerase Chain Reaction ; Rotavirus Infections ; Rotavirus* ; Sensitivity and Specificity

Viral respiratory infections are one of the most common infections worldwide. It is important to detect the virus early and precisely. In this study, we evaluated the limit of detection (LoD) and usefulness of the Real-Q RV Detection kit (BioSewoom, Seoul, Korea). We measured the LoD of the Real-Q RV Detection kit using 10 strains of standard viruses. We then compared the detection results by the Allplex Respiratory Panel Assay kit (Seegene, Seoul, Korea) using 123 clinical specimens. The discrepant results were confirmed by sequencing. Among the 10 standard viruses, the LoD of human rhinovirus (HRV) was the lowest and that of parainfluenza virus 2 and 3 was relatively high as detected by Real-Q RV Detection kit. Agreements of the two kits ranged from 95.9% to 100%. Three specimens detected negative by the Allplex Respiratory Panel kit were detected as adenovirus (AdV) by the Real-Q RV Detection kit and were confirmed by sequencing. Similarly, a specimen detected negative by the Allplex Respiratory Panel kit was detected as HRV by the Real-Q RV Detection kit and was confirmed by sequencing. A specimen detected as human enterovirus by the Allplex Respiratory Panel kit was detected as HRV by the Real-Q RV Detection kit and was confirmed by sequencing. Real-Q RV Detection kit showed good diagnostic performance and can be useful for detecting major viruses that cause respiratory infections.
Adenoviridae ; Enterovirus ; Humans ; Limit of Detection ; Paramyxoviridae Infections ; Respiratory Tract Infections* ; Rhinovirus ; Seoul

Enterococcus spp. are opportunistic pathogens that cause lameness in broiler chickens, resulting in serious economic losses worldwide. Virulence of Enterococcus spp. is associated with several putative virulence genes including fsr, efm, esp, cylA, cad1, ace, gelE, and asa1. In this study, multiplex polymerase chain reaction (PCR) for the simultaneous detection of these virulence genes in Enterococcus spp. was developed, and detection limits for E. faecium, E. faecalis, and E. hirae were 64.0 pg/µL, 320.0 pg/µL, and 1.6 ng/µL DNA, respectively. Among 80 Enterococcus isolates tested, efm and cad1 were detected in all 26 E. faecium samples, and only cad1 was observed in E. hirae. Additionally, the presence of virulence genes in 25 E. faecalis isolates were 100% for cad1, 88.0% for gelE, 64.0% for fsr, 44.0% for asa1, 16.0% for cylA, and 4.0% for esp. No virulence genes were found in E. gallinarum isolates. A total of 49 isolates were resistant to tigecycline and to at least 2 different classes of antibiotics. The most prevalent resistance was to ciprofloxacin (73.5%), quinupristin/dalfopristin (55.1%), and tetracycline (49.0%). No strains were resistant to vancomycin or linezolid. This is the first multiplex PCR assay to simultaneously detect eight virulence genes in Enterococcus spp., and the method provides diagnostic value for accurate, rapid, and convenient detection of virulence genes. Additionally, we report the prevalence of virulence genes and antimicrobial resistance in Enterococcus isolates from commercial broiler chickens suffering lameness.
Anti-Bacterial Agents ; Chickens ; Ciprofloxacin ; DNA ; Drug Resistance, Microbial ; Enterococcus ; Limit of Detection ; Linezolid ; Methods ; Multiplex Polymerase Chain Reaction ; Prevalence ; Tetracycline ; Vancomycin ; Virulence