[Determination of fatty acid composition after saponification of common oil pharmaceutical excipients by supercritical fluid-evaporative light scattering method and its application in oil identification].

Oils and fats are commonly used in the pharmaceutical industry as solvents, emulsifiers, wetting agents, and dispersants, and are an important category of pharmaceutical excipients. Fatty acids with unique compositions are important components of oil pharmaceutical excipients. The Chinese Pharmacopoeia provides clear descriptions of the fatty acid types and limits suitable for individual oil pharmaceutical excipient. An unqualified fatty acid composition or content may indicate adulteration or deterioration. The fatty acid composition, as a key indicator for the identification and adulteration evaluation of oil pharmaceutical excipients, can directly affect the quality and safety of oil pharmaceutical excipients and preparations. Gas chromatography is the most widely used technique for fatty acid analysis, but it generally requires derivatization, which affects quantitative accuracy. Supercritical fluid chromatography (SFC), an environmentally friendly technique with excellent separation capability, offers an efficient method for detecting fatty acids without derivatization. Unlike other chromatographic methods, SFC does not use nonvolatile solvents (e. g., water) as the mobile phase, rendering it compatible with an evaporative light-scattering detector (ELSD) for enhanced detection sensitivity. However, the fatty acids in oil pharmaceutical excipients exist in the free and bound forms, and the low content of free fatty acids in these oil pharmaceutical excipients not only poses challenges for their detection but also complicates the determination of characteristic fatty acid compositions and contents. Moreover, the compositions and ratios of fatty acids are influenced by environmental factors, leading to interconversion between their two forms. In this context, saponification provides a simpler and faster alternative to derivatization. Saponification degrades oils and fats by utilizing the reaction between esters and an alkaline solution, ultimately releasing the corresponding fatty acids. Because this method is more cost effective than derivatization, it is a suitable pretreatment method for the detection of fatty acids in oil pharmaceutical excipients using the SFC-ELSD approach. In this study, we employed SFC-ELSD to simultaneously determine six fatty acids, namely, myristic acid, palmitic acid, stearic acid, arachidic acid, docosanoic acid, and lignoceric acid, in oil pharmaceutical excipients. Saponification of the oil pharmaceutical excipients using sodium hydroxide methanol solution effectively avoided the bias in the determination of fatty acid species and contents caused by the interconversion of fatty acids and esters. The separation of the six fatty acids was achieved within 12 min, with good linearity within their respective mass concentration ranges. The limits of detection and quantification were 5-10 mg/L and 10-25 mg/L, respectively, and the spiked recoveries were 80.93%-111.66%. The method proved to be sensitive, reproducible, and stable, adequately meeting requirements for the analysis of fatty acids in oil pharmaceutical excipients. Finally, the analytical method was successfully applied to the determination of six fatty acids in five types of oil pharmaceutical excipients, namely, corn oil, soybean oil, coconut oil, olive oil, and peanut oil. It can be combined with principal component analysis to accurately differentiate different types of oil pharmaceutical excipients, providing technical support for the rapid identification and quality control of oil pharmaceutical excipients. Thus, the proposed method may potentially be applied to the analysis of complex systems adulterated with oil pharmaceutical excipients.

Effect of Shugan Tiaoshen acupuncture combined with western medication on depression-insomnia comorbidity due to COVID-19 quarantine: a multi-central randomized controlled trial / 中国针灸

OBJECTIVE@#To observe the effect of Shugan Tiaoshen acupuncture (acupuncture for soothing the liver and regulating the mentality) combined with western medication on depression and sleep quality in the patients with depression-insomnia comorbidity due to COVID-19 quarantine, and investigate the potential mechanism from the perspective of cortical excitability.@*METHODS@#Sixty patients with depression-insomnia comorbidity due to COVID-19 quarantine were randomly divided into an acupuncture group and a sham-acupuncture group, 30 cases in each one. The patients of both groups were treated with oral administration of sertraline hydrochloride tablets. In the acupuncture group, Shugan Tiaoshen acupuncture was supplemented. Body acupuncture was applied to Yintang (GV 24+), Baihui (GV 20), Hegu (LI 4), Zhaohai (KI 6), Qihai (CV 6), etc. The intradermal needling was used at Xin (CO15), Gan (CO12) and Shen (CO10). In the sham-acupuncture group, the sham-acupuncture was given at the same points as the acupuncture group. The compensatory treatment was provided at the end of follow-up for the patients in the sham-acupuncture group. In both groups, the treatment was given once every two days, 3 times a week, for consecutive 8 weeks. The self-rating depression scale (SDS) and insomnia severity index (ISI) scores were compared between the two groups before and after treatment and 1 month after the end of treatment (follow-up) separately. The cortical excitability indexes (resting motor threshold [rMT], motor evoked potential amplitude [MEP-A], cortical resting period [CSP]) and the level of serum 5-hydroxytryptamine (5-HT) were measured before and after treatment in the two groups.@*RESULTS@#After treatment and in follow-up, SDS and ISI scores were decreased in both groups compared with those before treatment (P<0.05), and the scores in the acupuncture group were lower than those in the sham-acupuncture group (P<0.05), and the decrease range in the acupuncture group after treatment was larger than that in the sham-acupuncture group (P<0.05). After treatment, rMT was reduced (P<0.05), while MEP-A and CSP were increased (P<0.05) in the acupuncture group compared with that before treatment. The levels of serum 5-HT in both groups were increased compared with those before treatment (P<0.05). The rMT in the acupuncture group was lower than that in the sham-acupuncture group, while MEP-A and CSP, as well as the level of serum 5-HT were higher in the acupuncture group in comparison with the sham-acupuncture group (P<0.05).@*CONCLUSION@#Shugan Tiaoshen acupuncture combined with western medication can relieve depression and improve sleep quality in the patients with depression-insomnia comorbidity due to COVID-19 quarantine, which is probably related to rectifying the imbalanced excitatory and inhibitory neuronal functions.

Surgical repair of an emergent giant hepatic aneurysm with an abdominal aortic dissection: A case report.

BACKGROUND: Hepatic artery aneurysm (HAA) is the second most common visceral aneurysm. A significant number of hepatic aneurysms are found accidentally on examination. However, their natural history is characterized by their propensity to rupture, which is very serious and requires urgent treatment. An emergent giant hepatic aneurysm with an abdominal aortic dissection is less commonly reported. CASE SUMMARY: We report the complicated case of a giant hepatic aneurysm with an abdominal aortic dissection. A 66-year-old female presented with the complaint of sudden upper abdominal pain accompanied by vomiting. Physical examination showed that her blood pressure was 214/113 mmHg. Her other vital signs were stable. Computed tomography found a giant hepatic proper aneurysm and dissection of the lower segment of the abdominal aorta. Furthermore, angiography showed a HAA with the maximum diameter of approximately 56 mm originating from the proper hepatic artery and located approximately 15 mm from the involved bifurcation of the left and right hepatic arteries with no collateral circulation. Therefore, we decided to use a stent to isolate the abdominal aortic dissection first, and then performed open repair. After the operation, the patient recovered well without complications, and her 3-month follow-up checkup did not reveal any late complications. CONCLUSION: Open surgery is a proven method for treating giant hepatic aneurysms. If the patient's condition is complex, staged surgery is an option.

The clinical and radiological features of myelin oligodendrocyte glycoprotein antibody associated disease / 中华神经科杂志

Objective@#To explore the clinical and radiological features of myelin oligodendrocyte glycoprotein (MOG) antibody associated disease.@*Methods@#The clinical data of 22 MOG antibody associated disease cases treated in the Department of Neurology, Qilu Hospital of Shandong University from January 2017 to June 2019 were retrospectively analyzed. The clinical data of MOG antibody associated disease were summarized, including clinical and imaging features.@*Results@#Of the 22 included patients with MOG antibody associated disease, the average age was 38.5 years, 13 were male and nine were female. Among them, 11 cases manifested as aquaporin-4 (AQP4)-negative neuromyelitis optica spectrum disorder (NMOSD), four cases optic neuritis, two cases transverse myelitis, one case acute disseminated encephalomyelitis (ADEM), two cases cortical encephalitis and two cases vestibular neuronitis. Magnetic resonance imaging (MRI) results showed that multiple anatomical areas were involved. Among the nine patients with optic nerve involvement, five patients had longitudinally extensive optic nerve lesions, which were longitudinally enhanced. In eight patients, MRI lesions in the spinal cord showed mostly long or short segments involvement, involving 2-5 spinal cord segments. Five cases involved the cervical spinal cord, six cases involved the thoracic spinal cord, and one case involved the lumbar spinal cord. Brain MRI abnormalities were found in 13 cases and the lesions were mostly patchy and point-shaped. MRI lesions demonstrated T2 hyperintensity and some of them could be strengthened, which may involve the basal ganglia, thalamus, radiographic crown, frontal temporal lobe, brain stem and other parts. Among them, 16 patients were sensitive to high-dose intravenous/oral methylprednisolone in the acute phase. Seven patients had recurrence after two months to two years of follow-up.@*Conclusions@#MOG antibody associated disease include multiple manifestations. Among them, AQP4-negative NMOSD is the most common form. The clinical manifestations of patients showed diversity. Imaging is characterized by multiple parts involvement such as optic nerve, spinal cord, and brain. Most patients are sensitive to high-dose intravenous/oral methylprednisolone, and have a good prognosis in the acute phase, but some patients may relapse.

The clinical and radiological features of superficial siderosis of central nervous system: report of four cases / 中华神经科杂志

Objective:To explore the etiology, clinical features and treatment of superficial siderosis of central nervous system (SSCNS) in China.Methods:The clinical data of four patients with SSCNS diagnosed by magnetic resonance imaging (MRI) and susceptibility weighted imaging (SWI) from Qilu Hospital of Shandong University during 2015—2019 were retrospectively reviewed. The etiology and clinical features of the four cases were summarized and analyzed.Results:All the four patients were male, with an average age of 60.5 years. Clinical symptoms included headache, hearing loss, and cerebellar ataxia. Brain MRI and SWI showed that hemosiderin mainly deposited (short linear T 2 signal, low SWI signal) on the surface of cerebellum, brainstem, temporal lobe, frontal lobe, and spinal cord. Potential bleeding sites were found in all four patients, including brain traumatic history, spinal intradural extramedullary cavernous hemangioma, brain metastasis and intracranial aneurysm. Patients were followed up for six months to four years. Headache symptoms improved in only one patient who received surgical treatment, while symptoms of the other three patients progressed. Conclusions:SSCNS is mainly characterized by hearing loss, progressive cerebellar ataxia and myelopathy. The diagnosis of this disease mainly depends on imaging examination. The linear low signal on the surface of T 2WI is the main basis for the diagnosis of SSCNS. Surgical treatment of bleeding sites and iron chelator are the main treatments of the disease.

The clinical and radiological features of myelin oligodendrocyte glycoprotein antibody associated disease / 中华神经科杂志

Objective To explore the clinical and radiological features of myelin oligodendrocyte glycoprotein (MOG) antibody associated disease.Methods The clinical data of 22 MOG antibody associated disease cases treated in the Department of Neurology,Qilu Hospital of Shandong University from January 2017 to June 2019 were retrospectively analyzed.The clinical data of MOG antibody associated disease were summarized,including clinical and imaging features.Results Of the 22 included patients with MOG antibody associated disease,the average age was 38.5 years,13 were male and nine were female.Among them,11 cases manifested as aquaporin-4 (AQP4)-negative neuromyelitis optica spectrum disorder (NMOSD),four cases optic neuritis,two cases transverse myelitis,one case acute disseminated encephalomyelitis (ADEM),two cases cortical encephalitis and two cases vestibular neuronitis.Magnetic resonance imaging (MRI) results showed that multiple anatomical areas were involved.Among the nine patients with optic nerve involvement,five patients had longitudinally extensive optic nerve lesions,which were longitudinally enhanced.In eight patients,MRI lesions in the spinal cord showed mostly long or short segments involvement,involving 2-5 spinal cord segments.Five cases involved the cervical spinal cord,six cases involved the thoracic spinal cord,and one case involved the lumbar spinal cord.Brain MRI abnormalities were found in 13 cases and the lesions were mostly patchy and point-shaped.MRI lesions demonstrated T2 hyperintensity and some of them could be strengthened,which may involve the basal ganglia,thalamus,radiographic crown,frontal temporal lobe,brain stem and other parts.Among them,16 patients were sensitive to high-dose intravenous/oral methylprednisolone in the acute phase.Seven patients had recurrence after two months to two years of follow-up.Conclusions MOG antibody associated disease include multiple manifestations.Among them,AQP4-negative NMOSD is the most common form.The clinical manifestations of patients showed diversity.Imaging is characterized by multiple parts involvement such as optic nerve,spinal cord,and brain.Most patients are sensitive to high-dose intravenous/oral methylprednisolone,and have a good prognosis in the acute phase,but some patients may relapse.

Advances in the Components Analysis of Aminoglycosides / 中国药学杂志

This paper first briefly introduces the basic information of aminoglycosides for pharmaceutical use such as origin, classification, chemical structures, diversity of composition and the research originators, etc. Then it reviews the development process of the technologies for the analysis of components of aminoglycosides, discusses the advantages and disadvantages of current methodologies and explains the advantage of liquid chromatography coupled with pulsed amperometric detection method for analysis of the components of aminoglycosides. At last, it introduces some new analysis technologies and ideas and forecasts the direction of future development.

[Curative effect of anti-HBV treatment in advanced schistosomiasis patients with ascites and HIBV infection].

OBJECTIVE: To improve the curative effect of advanced schistosomiasis patients with ascites and HBV infection. METHODS: A total of 27 advanced schistosomiasis patients with ascites and HBV infection were selected as a trial group and given with anti-HBV treatment, and 31 corresponding patients were as the controls and did not received anti-HBV treatment from February 2003 to December 2012. RESULTS: The incidence of ascites recurrence, spontaneous peritonitis, hepatic encephalopathy, hepatorenal syndrome, upper gastrointestinal bleeding, and primary liver cancer in the trial group were significantly lower than those in the control group. The detection indexes of liver function, renal function and prothrombin time in the trial group were superior to those in the control group. The mortality in the treatment group was also significantly lower than that in the control group. CONCLUSION: The anti-HBV treatment in the advanced schistosomiasis patients with ascites and HBV infection can obviously improve their physical conditions, the survival rate, and their life qualities.

Identification of the related substances in etimicin sulfate detected under the condition of Chinese Pharmacopoeia 2010 by LC/MSn with propionic acid enhanced electrospray ionization / 中国药学杂志

OBJECTIVE: To establish an LC/MSn method for identification of the related substances in etimicn sulfate detected under the chromatographic condition described in Chinese Pharmacopoeia 2010. METHODS: The HPLC separation was carried out on a Welch Ultimate LP-C18 column (4.6 mm × 300 mm, 5 μm) with mobile phase consisting of 0.2 mol · L-1 trifluoroacetic acid (containing 0.1% propionic acid ) -methanol (84: 16) at a flow rate of 1.0 mL · min-1. Thirty percent of the eluent was detected by ion trap mass spectrometry, and the parent ions and the corresponding product spectra of all the related substances in etimicin sulfate were determined and elucidated. RESULTS: Addition of 0.1% propionic acid into the mobile phase significantly enhanced the sensitivity of MS detector without altering the chromatographic behavior such as retention time and elution order of the related substances. Twenty-eight related substances were separated and detected by the LC/MSn method in a typical sample. Nine of them were identified with the help of corresponding impurity reference substances and 14 of them were elucidated by MS fragment information, while the other five were not identified due to limitated information. CONCLUSION: The established method can be applied to the identification of the related substances in etimicn sulfate detected under the chromatographic condition described in Chinese Pharmacopoeia 2010, which is helpful to the quality improvement and process optimization of etmicin sulfate.

[Long-term therapeutic effect of Ruangan pills on advanced schistosomiasis patients with ascites].

OBJECTIVE: To evaluate the long-term therapeutic effect of Ruangan pills on advanced schistosomiasis combined with ascites. METHODS: The data of 54 advanced schistosomiasis patients with ascites were collected, and the patients were divided into two groups namely a treatment group and a control group according to whether taking Ruangan pills. The effective rates, improvement status of symptoms and levels of serum albumin (ALB) and hyaluronic acid (HA) of the two groups were compared. RESULTS: The effective rates of the treatment group and control group were 92.59% and 44.44%, respectively, and the difference between them was statistically significant (P < 0.05). After the treatment for 9 and 12 months, the percentages of patients without ascites and patients with symptom improvement in the treatment group were 77.78% and 92.59%, 92.59% and 96.30%, respectively, while those in the control group were 29.63% and 37.00%, 48.15% and 51.85%, respectively, and the differences between the two groups by different time were all statistical significant (all P < 0.05). After the treatment for 9 months, the percentages of patients with the normal levels of ALB and HA were 88.89% and 59.26%, while those in the control group were 40.74% and 14.81%, respectively, and the differences between the two groups were statistically significant (both P < 0.05). CONCLUSION: The long-term treatment of Ruangan pills can not only improve clinical symptoms but also control the ascites recurrence, however, the therapeutic effect and the recurrence rate of ascites in longer-term still need further observation.

Analysis of impurities in vertilmicin sulfate by liquid chromatography ion-trap mass spectrometry.

The characterization of impurities present in vertilmicin by liquid chromatography (LC) coupled with mass spectrometry (MS) is described. A reversed phase (RP)-LC method using a C18 column resistant to basic pH with an alkaline (pH 11) aqueous mobile phase was developed and coupled to MS with an electrospray ionization (ESI) source in the positive ion mode which provides MS(n) capability. In total, 18 impurities were detected in a commercial sample. Eleven impurities described in this work were newly identified.

Impurity profiling of micronomicin sulfate injection by liquid chromatography-ion trap mass spectrometry.

The characterization of impurities present in micronomicin sulfate injection by liquid chromatography (LC) coupled with mass spectrometry (MS) is described. A reversed phase (RP)-LC method using a C18 column resistant to an alkaline (pH 11) aqueous mobile phase was developed and coupled to MS with an electrospray ionization (ESI) source in the positive ion mode which provides MS(n) capability. A total of thirty six impurities were detected in commercial samples: five impurities were identified by comparison of their fragmentation patterns with those of available related substances, eleven of them were identified in accordance with relevant literature, while the other twenty impurities were newly identified using the MS/MS spectra of the available related reference substances as interpretative templates combined with knowledge of the nature of functional group fragmentation behaviors. This work was applied to evaluate the quality of micronomicin sulfate injection from different manufacturers.

Effect of video-assisted thoracoscopic surgery in thoracic disease / 局解手术学杂志

Objective To investigate the effect of video-assisted thoracoscopic surgery( VATS) in thoracic disease,and the feasibility to carry out VATS for basic hospital. Methods The data of VATS treatment were collected to compare the differences between study group and control group,and evaluate the the feasibility to carry out VATS for basic hospital. Results The operation time was (100. 75±22. 72) min, blood loss was (54. 27±26. 21) mL,postoperative drainage was (920. 67±171. 99) mL. The postoperative complications were fewer,post-operative hospital stay was shorter,incision time was shorter(P=0. 000) and pain scores was lower(P=0. 000) in study group than that in control group. Basic hospital has the capacity to conduct this technical. Conclusion VATS is feasible to carry out in basic hospital.

Impurity profiling of etimicin sulfate by liquid chromatography ion-trap mass spectrometry.

A reversed phase (RP)-LC method using a C(18) column resistant to basic pH and an alkaline (pH 10) aqueous mobile phase was developed and coupled to MS with an electrospray ionization (ESI) source in the positive ion mode which provides MS(n) capability. In total, 26 impurities were detected in a commercial sample. The structures of the impurities were proposed based on comparison of their fragmentation patterns with those of the available reference substances, the synthetic route and literature data. Starting material and its residual impurities, intermediates, synthetic by-products and degradation products were the main sources of those impurities. 14 impurities described in this work were newly identified.

[Related substances in purified alliin determined by HPLC-MS/MS].

To study the related substances in purified alliin, HPLC-MS/MS method carried out on a Phenomenex NH2 column was used for screen and identification of the related substances with full scan MS spectra determination of their [M + H] + ions and then the analyses of the retention time, product MS spectra and/or chemical reference standards. The full scan HPLC-MS chromatogram showed that there were seven major related substances in the purified alliin and their m/z of the [M + H] + ions with increasing retention were 116, 133, 147, 152, 175, 178 and 178, separately. And they were identified as proline, asparagine, glutamine, methiin, arginine, isoalliin and cycloalliin (both were isomers of alliin), respectively. The major related substances in purified alliin are amino acids, homologen and the isomers of alliin.

Related substances in purified alliin determined by HPLC-MS/MS / 药学学报

To study the related substances in purified alliin, HPLC-MS/MS method carried out on a Phenomenex NH2 column was used for screen and identification of the related substances with full scan MS spectra determination of their [M + H] + ions and then the analyses of the retention time, product MS spectra and/or chemical reference standards. The full scan HPLC-MS chromatogram showed that there were seven major related substances in the purified alliin and their m/z of the [M + H] + ions with increasing retention were 116, 133, 147, 152, 175, 178 and 178, separately. And they were identified as proline, asparagine, glutamine, methiin, arginine, isoalliin and cycloalliin (both were isomers of alliin), respectively. The major related substances in purified alliin are amino acids, homologen and the isomers of alliin.

[Study on water of crystallization in tazobactam].

AIM: To investigate whether tazobctam has crystallization water. METHODS: In order to establish a method for water content determination in tazobctam, many methods including Karl Fischer titration, weight loss on drying, TGA, DSC and X-ray diffraction experiment of an orthorhombic form were studied. RESULTS: The water content of the same batch tazobactam determined by different mthods was different. CONCLUSION: The results showed that one mole tazobatam contains half mole water of crystallization and the strength of attraction between tazobatam molecule and water molecule is rather strong.

Study on water of crystallization in tazobactam / 药学学报

<p><b>AIM</b>To investigate whether tazobctam has crystallization water.</p><p><b>METHODS</b>In order to establish a method for water content determination in tazobctam, many methods including Karl Fischer titration, weight loss on drying, TGA, DSC and X-ray diffraction experiment of an orthorhombic form were studied.</p><p><b>RESULTS</b>The water content of the same batch tazobactam determined by different mthods was different.</p><p><b>CONCLUSION</b>The results showed that one mole tazobatam contains half mole water of crystallization and the strength of attraction between tazobatam molecule and water molecule is rather strong.</p>