摘要
A derivatizaton method combined with gas chromatography-mass spectrometry(GC-MS)was established for detection of isobutyl chloroformate(IBCF)residue in active pharmaceutical ingredient of agatroban.The extraction and derivatization reagents,derivatization time,qualitative and quantitative ions were selected and optimized,respectively.The possible mechanism of derivatization and characteristic fragment ions fragmentation were speculated.The agatroban samples were dissolved and extracted by methanol,and the residual IBCF was derived with methanol to generate methyl isobutyl carbonate(MIBCB).After 24 h static derivatization at room temperature,IBCF was completely transformed into MIBCB,which could be used to indirectly detect IBCF accurately.The results showed that the linearity of this method was good in the range of 25-500 ng/mL(R2=0.9999).The limit of detection(LOD,S/N=3)was 0.75 μg/g,and the limit of quantification(LOQ,S/N=10)was 2.50 μg/g.Good recoveries(95.2%-97.8%)and relative standard deviations(RSDs)less than 3.1%(n=6)were obtained from agatroban samples at three spiked levels of IBCF(2.50,25.00,50.00 μg/g),which showed good accuracy of this method.Good precision of detection results was obtained by different laboratory technicians at different times,the mean value of spiked sample solution(25.00 μg/g)was 24.28 μg/g,and the RSD was 2.1%(n=12).The durability was good,minor changes of detection conditions had little effect on the results.Under the original condition and conditions with initial column temperature±5℃,heating rate±2℃/min,column flow rate±0.1 mL/min,the IBCF content of spiked sample solution(25.00 μg/g)was detected,the mean value of detection results was 24.16 μg/g,and the RSD was 2.2%(n=7).Eight batches of agatroban samples from two manufacturers were detected using the established method,and the results showed that no IBCF residue was detected in any of these samples.The agatroban samples could be dissolved by methanol,and then the IBCF residue could be simultaneously extracted and derived with methanol as well.This detection method had the advantages of simple operation,high sensitivity,low matrix effect and accurate quantification,which provided a new effective method for detection of IBCF residue in agatroban.
摘要
Objective To investigate the clinical significance of monitoring the renal pelvic pressure( RPP) and regulating the manual perfusion pressure in flexible ureteroscope holmium laser lithotripsy. Methods A total of 189 patients with upper urinary tract calculi treated by RIRS in our hospital were retrospectively analyzed from August 2014 to August 2017. The renal pelvic pressure was monitored during RIRS in 136 cases( monitored group) whereas no monitoring occurred in the rest 53 cases( unmonitored group) . The monitored group was divided into two sub-groups of 49 cases named high-pressure group(the cumulative time of renal pelvis pressure upon 40 cmH2O≥1 min) and 87 ca-ses named low-pressure group respectively. The morbidity of postoperative fever ( T≥38. 5℃) was evaluated statistically between monitored group and unmonitored group,meanwhile between high-pressure group and low-pressure group. Results Postoperative fever did not correlate to age,sex,involved kidney,and postoperative urinary tract infection. Whether renal pelvic pressure was monitored or not,infection calculi, duration of operation and whether the cumulative time of renal pelvis pressure upon 40cmH2O≥1 min contributed to postoperative fever. The rate of postoperative fever in unmonitored group was higher than monitored group while the same between high-pressure group and low-pres-sure group,with statistically significant difference(P<0. 05). Conclusion Monitoring the intraoperative RRP and regulating the manual perfusion pressure during RIRS has positive significance in postoperative recovery and contribute to reducing postoperative fever.
摘要
[Objective] To investigate the purchase and use of edible oil , as well as recycling of kitchen waste oil in Shanghai catering service units , providing reference for relevant regulatory authorities . <br> [ Methods] A total of 976 units of various types of catering service in Shanghai were selected via strati-fied sampling methodology , a self-designed questionnaire used to investigate the purchase and use of edi-ble oil, as well as recycling of kitchen waste oil .Meanwhile, an on-site rapid detection technology was used to test items including acid value , peroxide value , polar components of unused pre -packaged edible oil and also the process of using frying oils on site . [ Results] The amount of edible oil used in catering service units of Shanghai was about 1235 tons per day;6.0% of the oil purchased was bulk cooking oil , which accounted for 5 .6%of the total amount consumed;44 .3%of the catering service units signed with professional companies for the recycling of kitchen waste oil;3615 samples were detected using an on -site rapid detection , of which 17 were suspected to be positive .The lab confirmed that test results were quali-fied. [ Conclusion] The edible oil used in Shanghai catering service units is safe in general , while bulk cooking oil may have potential safety hazards .Food practitioners have low awareness of health risk caused <br> by using edible oil repeatedly and for too long time , which makes some enterprise use “old oil” for too long;There does exist the possibility of kitchen waste oil returning to food chain as its recycling has not been standardized .
摘要
<p><b>OBJECTIVE</b>To explore the feasibility of urethroplasty with transection of the urethral orifice and preservation and lengthening of the urethral plate in the treatment of hypospadias.</p><p><b>METHODS</b>Forty-eight patients with hypospadias (18 of the coronal type, 21 the penile type, 8 the penoscrotal type and 1 the perineal type) underwent urethroplasty with transection of the urethral orifice and preservation and lengthening of the urethral plate. The surgical effects were observed by following up the patients for 3-27 months.</p><p><b>RESULTS</b>One-stage surgical success was achieved in 44 of the cases, with satisfactory functional and cosmetic results but no complications. Two cases developed urinary fistula and another 2 urethral stricture, but all cured by the second surgery.</p><p><b>CONCLUSION</b>Urethroplasty with transection of the urethral orifice and preservation and lengthening of the urethral plate is a simple, safe and effective surgical procedure for the treatment of hypospadias.</p>