Proficiency testing for psychoactive substances in Italy

This paper describes the general design and main results of the Italian proficiency testing program for the analysis of psychoactive substances in urine, a long-term initiative created in 1995 on an educational basis and characterized by an innovative internet-based service for data exchange between laboratories and the organizing body. Batches of six urine samples, validated by reference laboratories, are sent every 3 months to participating laboratories, which may choose which classes of substances to test from those planned by the program panel and, within those classes, which type of analytical commitment to work on: identification of just one class (Option 1), identification of single substances (Option 2), or identification and quantification of single substances (Option 3). Comprehensive periodical reports and annual reports are provided to participants with evaluation of their performance and an annual workshop is organized to discuss technical-scientific topics related to clinical, forensic and analytical toxicology. About 200 laboratories currently participate in the program and a total of 67,059 analyses have been carried out since 1995. The mean percentage of correct results was 96.8%, with a yearly improvement of about 0.4%. The best average false positive and false negative rates were obtained for methadone (0.2% and 2.1% respectively) and cocaine (0.3% and 2.2%). The worst average false positive rates were obtained for amphetamines and opiates (3.2% and 5.0%) and worst average false negative rates for amphetamines, barbiturates and cannabinoids (17.4%, 30.7% and 19.9%). Received: 29 June 1998 / Received in revised form: 23 February 1999     

Circadian rhythm of lithogenic substances in the urine

Summary After determination of the lithogenic and inhibitory substances in serum and urine of 18 healthy control subjects and 20 patients with calcium oxalate urolithiasis on an uncontrolled diet, the alteration of the parameters while taking a standard diet was investigated. After attainment of a steady state, the investigations were performed over 48h on 3-h aliquots of urine. Typical circadian rhythms were detected for all lithogenic parameters in the urine and normal ranges were established. This special investigation permits detection of peaks in the excretion of lithogenic substances which were masked in investigation of 24-h urine samples alone.     

用HPLC法测定马来酸依那普利片的含量和有关物质

目的:采用改进的HPLC法测定马来酸依那普利片中马来酸依那普利和有关物质的含量。方法:采用HypersilBDS C8色谱柱(250 mm×4.0 mm,5μm ID);0.001 mol/L磷酸二氢铵溶液(用磷酸调节pH值至2.0)-甲醇(60:40);检测波长215 nm。结果:马来酸依那普利在0.1～0.3 mg/ml范围内线性关系良好(r=0.999 9);方法的平均回收率为99.8％。依那普利与有关物质之间分离良好。结论:本法有较高的回收率、精密度和重现性。     

我院门诊病人处方中精神药品药物利用调查分析

目的 :了解我院精神药品 (psychotropicsubstances)使用情况 ,促进合理用药。方法 :采用限定日剂量和药物利用指数为指标对我院门诊精神药品的处方进行调查和分析。结果 ;平均药物利用指数在 1.0 0左右 ,用药时间大于 4wk的达 79.0 9% ,合并用药大于 2种药物的占 13.14 %。结论 :我院精神药品的使用基本合理 ,但用药时间较长 ,合并用药频度较高     

肠三叶因子对新生鼠缺氧肠损伤模型白细胞介素8、丙二醛的影响及意义

目的　研究肠三叶因子 (intestinaltrefoilfactor,ITF)对坏死性小肠结肠炎 (necrotizingenterocolitis,NEC)新生大鼠的肠粘膜中白细胞介素 8(interleukin 8,IL 8)及丙二醛 (malondialdehyde,MDA)含量的影响 ,探讨ITF对NEC是否有保护作用。　方法　建立NEC模型 ,对新生 1日龄Wistar大鼠予 10 0 %二氧化碳 ,5min后再予 10 0 %氧气 ,5min后放回母鼠身边喂养 ,第 4天处死大鼠取肠道组织待检。新生鼠 32只随机分为四组 ,A组为NEC模型后腹腔注射ITF 0 .5mg ;B组为NEC模型后皮下注射ITF 0 .2mg ;C组为NEC模型组 ;D组为正常对照组。取近回盲段 1～ 2cm肠道组织固定包埋、切片、HE染色光镜下作病理学检查 ,其他肠道组织制备组织匀浆取上清液用放射性免疫法检测IL 8,用生化法检测MDA的含量。　结果　A、B组IL 8的含量 [pg (mg·pro) ]各为 2 9.72 2± 7.134、30 .5 12± 8.2 30 ,均较C组 39.379± 4 .4 2 0低 (P <0 .0 5 ) ,而与D组 2 3.92 2± 6 .16 8比较 ,差异无显著性 (P >0 .0 5 ) ;A、B组MDA的含量 [nmol (mg·pro) ]各为 2 .2 6 7± 0 .2 6 7、2 .15 4± 0 .30 1,较C组 3.378± 0 .835低 (P <0 .0 1) ,与D组 2 .2 2 5± 0 .4 4 3比较 ,差异无显著性 (P >0 .0 5 )。C组HE染色切片见肠壁的损伤轻重不一 ,有的     

HPLC法测定硝呋拉呔的含量及有关物质的方法学研究

目的:采用高效液相色谱法测定硝呋拉呔的含量及有关物质。方法:采用ODSC_(18)色谱柱(5μm,4.6mm×250mm),以甲醇-水(45:55)为流动相,流速1.2 mL·min~(-1),紫外检测器于254 nm测定。结果:HPLC法测定的线性范围为0.01～0.4mg·mL~(-1),r=0.999 9,最低检测限0.2 ng;样品溶液在8 h内稳定,日内精密度和日间精密度(RSD<1.0％)良好。回收率为100.1％。结论:采用HPLC法测定硝呋拉呔及有关物质的方法简便,结果可靠。     

离子抑制色谱法测定琥乙红霉素含量及其有关物质

目的　建立离子抑制色谱法测定琥乙红霉素原料的含量及有关物质的方法 ,并研究其影响因素。方法　采用ZorbaxSB -C1 8色谱柱 ,以 0 .0 2mol·L- 1 KH2 PO4 乙腈 ( 4 5∶5 5 ,用氨试液调至pH 6 .8)为流动相 ,流速 1.2mL·min- 1 ,检测波长 2 10nm ,柱温 ( 30± 0 .5 )℃。结果　在选定固定相条件下 ,流动相对组分的洗脱和选择性影响最大 ,柱温次之 ,琥乙红霉素在乙腈中比较稳定。测定了有效主成分琥乙红霉素A的含量以及 7个有关物质的总含量 ,琥乙红霉素A的平均回收率为 99.4 5 %(RSD =2 .2 4 % ,n =5 )。结论　本方法可用于琥乙红霉素原料的含量测定和有关物质的检查。     

HPLC法测定头孢羟氨苄及其有关物质含量

目的建立头孢羟氨苄有关物质的HPLC分析方法。方法采用ODS柱(Polaris250mm×4.6mm,5μm),以0.05mol/L磷酸盐缓冲液(用10mol/L氢氧化钾调节pH值为5.5)-乙腈(96∶4)为流动相,流速为0.7ml/min,检测波长为230nm。结果头孢羟氨苄、有关物质α-对羟基苯甘氨酸、7-氨基去乙酰氧基头孢烷酸(7-ADCA)的线性范围分别为0.125～1.0mg/ml(r=0.9997)、0.312～20μg/ml(r=0.9999)、0.312～20μg/ml(r=0.9999)。结论本方法可用于头孢羟氨苄及其有关物质含量的测定,方法准确、灵敏、简便。     

聚甲酚磺醛溶液中4种有关物质的HPLC测定

目的:建立同时测定聚甲酚磺醛溶液中4种有关物质间甲酚-4,6-二磺酸、间甲酚-4-磺酸、间甲酚-6-磺酸及双甲酚磺酸的HPLC方法。方法:采用Diamonsil TMC18色谱柱(4.6 mm×250 mm,5 μm),以1％乙酸铵水溶液为流动相A,以甲醇为流动相B进行程序梯度洗脱,柱温30℃,检测波长280 nm,流速0.8 mL·min-1。结果:在选定的色谱条件下,4种有关物质均能得到较好的分离,在测定范围内具有良好的线性及精密度。结论:此方法简便、快速、准确,可用于聚甲酚磺醛溶液有关物质的测定。