Objective To develop a HPLC-MS/MS method for comprehensive monitoring and control of the raw material feeding (honeysuchle flowers extract and baikal skullcap root extract) , and simultaneous determination of chlorogenic acid and baicalin in Yinhuang capsules. Methods The separation was performed on an Inertsil ODS-3 (2.1 mm × 150 mm, 5 μm) analytical column with the mobile phase consisting of methanol- 10 mmol/L ammonium acetate solution by gradient elution program, and the column temperature was 40 ℃. Active ingredients were separated by HPLC, and the Electrospray Ionization Mass (API) source was applied and operated in the negative ion mode, and reactions ion monitoring mode (MRM) for quantitative analysis were selected. Results The samples and the mixed Extract have the same characteristic peak in MS and MS/MS. According to the prescription feeding process, the proprietary Chinese medicine wasdetermined. The results showed that the palladium residue of 6 batches samples were up to the standard by HPLC/MS/MS chromatographic peak areas. The calibration cruve of chlorogenic acid and baicalin were linear: 0.60-4.80 μg/ml (r = 0.9989),2.87-14.40 μg/ml (r = 0.9986), with the relative standard deviation of repeatability by 0.69% and 0.69% respectively, and the mean recovery rate were 95%-102%, 95%-103%, respectively. Conclusions The method was proven to be simple, accurate, reliable, high sensitive and can be used for determination and control of the raw material feeding (honeysuchle flowers extract and baikal skullcap root extract) and quality in Yinhuang capsules.

Objective To investigate the effect of the timing of endoscopic retrograde cholangiopancreatography(ERCP)treat-ment option on the respiratory burst and inflammatory factor level for acute obstructive suppurative cholangitis(AOSC)patients. Methods A total of 98 patients with AOSC who were treated in our hospital from January 2013 to June 2016 were retrospectively analyzed.The patients were divided into A group and B group according to the time of ERCP operation.42 cases in A group were received ERCP within 6 h after admission.56 cases in B group were received ERCP in 6-24 h after admission.,The serum levels of inflammatory cytokines were compared between the two groups before and after treatment.The apoptosis rate and respiratory burst rate of peripheral hematoma were compared between the two groups before and after treatment.The complications and death rate of the patients in the two groups were recorded.Results After treatment,the levels of TNF-α and IL-6 in the A group were signifi-cantly lower than those in the B group and the IL-10 level was significantly higher in the B group(P<0.05).After treatment,the rate of neutrophil apoptosis in the A group was significantly higher than that in the B group(P<0.05),and the respiratory burst level in the A group was significantly lower than that in the B group(P<0.05).The incidence number of complications and death in patients in group A was significantly lower than that in group B(P< 0.05).Conclusion ERCP treatment for patients with AOSC should be performed as early as possible and as soon as possible.Early ERCP treatment is safe and effective and can alleviate the inflammatory reaction of patients,improve the survival rate of patients,and is worthy of clinical promotion.

Objective The monitoring of the feeding situation of active pharmaceutical ingredient in Shendan-Chenpi tablet by HPLC-MS/MS,and the content of sodium taurocholate and hesperidin.Methods Using ZORBAX Eclipse Plus C18(4.6 mm×250 mm, 5 μm)Column temperature 40 ℃, Mobile phase with acetonitrile-10 mmol/sodium acetate solution, using gradient elution program. Active ingredients were separated by HPLC, and the Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode, and reactions ion monitoring mode(MRM) for quantitative analysis were selected. Results The proprietary Chinese medicine is judged by the prescription feeding process, through analysis and contrast of the medicinal materials, reference substance of primary mass spectrogram, secondary mass spectrogram of peak. The aurocholic acid sodium and hesperidin had a good linear relationship in 0.242×10-2-1.45×10-2μg(r=0.996 0), 0.688×10-2-10.30×10-2μg(r=0.999 2), and the precision test were 0.78% and 1.56%, and the recovery rate were 102%-103%,96%-109%. Conclusions The method was simple, accurate and reliable, high sensitive and fast. The comprehensive monitoring was applied to the Shedan-Chenpi tablet in feeding analysis and quality.

Background Exposure to perfluoroalkyl and polyfluoroalkyl substances (PFAS) during pregnancy might affect thyroid-related hormone levels in pregnant women. However, most previous studies focused on the effects of PFAS containing 8-10 carbon atoms, and few studies have estimated the associations between PFAS with longer carbon chain and thyroid-related hormone levels. Objective To examine the associations between PFAS exposure and thyroid-related hormones in pregnant women. Methods The present study was based on the Jiashan Birth Cohort from September 2016 to April 2018. We analyzed 13 PFAS in maternal blood samples (n=781) by high-performance liquid chromatography-tandem mass spectrometry, as well as total triiodothyronine (T3), total thyroxine (T4), free T3 (FT3), free T4 (FT4), thyroid stimulating hormone (TSH), thyroglobulin antibody (TG-Ab), and thyroid peroxidase antibody (TPOAb) by electrochemiluminescence immunoassay. PFAS were divided into three groups:low concentration, medium concentration and high concentration according to the tertile of their concentrations. We estimated the associations between PFAS concentrations and thyroid-related hormones in pregnant women by multiple linear regression. Results In the multiple linear regression models, a change in perfluorododecanoic acid (PFDoA) concentrations from the low concentration group to the high concentration group was associated with a −0.10 (95%CI: −0.20, 0) nmol·L⁻¹ change in T3, −0.15 (95%CI: −0.28, −0.02) pmol·L⁻¹ change in FT3, and −3.02 (95%CI: −5.66, −0.39) pmol·L⁻¹ change in FT4, respectively. A change in perfluorotridecanoic acid (PFTrDA) concentrations from the low concentration group to the high concentration group was associated with a −0.10 (95%CI: −0.20, 0) nmol·L⁻¹ change in T3. Compared with the low concentration group, the concentration of T4 in the medium concentration group of perfluorohexane sulfonate (PFHxS) increased by 6.10 (95%CI: 0.44, 11.75) nmol·L⁻¹. No statistically significant associations were found between PFAS and TSH concentration. The negative associations of PFAS with thyroid-related hormones were more pronounced in pregnant women with positive TG-Ab and/or TPOAb. Conclusion Exposure to PFAS during pregnancy may affect thyroid-related hormone homeostasis in pregnant women, and the effect is stronger in TG-Ab and/or TPOAb-positive pregnant women.