应用超高效液相色谱-串联质谱法测定了助眠类保健品中22种禁用安神类药物的含量。将样品连同其包衣和胶囊壳一起研碎后称取1.000g样品用甲醇溶解,经涡旋混匀并超声15min,用甲醇定容至25.0mL。离心后取上清液5.00mL,经Oasis PRiME HLB固...应用超高效液相色谱-串联质谱法测定了助眠类保健品中22种禁用安神类药物的含量。将样品连同其包衣和胶囊壳一起研碎后称取1.000g样品用甲醇溶解,经涡旋混匀并超声15min,用甲醇定容至25.0mL。离心后取上清液5.00mL,经Oasis PRiME HLB固相萃取柱净化处理,收集经净化的流出液,与用于淋洗固相萃取柱的甲醇2mL合并,于40℃下吹氮至溶液近干。用体积比为1∶1的0.05%(体积分数,下同)甲酸-甲醇混合溶液1.00mL溶解残渣,所得溶液经过0.22μm滤膜过滤,滤液供色谱分离。选用Poroshell 120EC-C18色谱柱(50mm×3.0mm,2.7μm)作为固定相,用不同比例的(A)含0.05%甲酸的5mmol·L^-1乙酸铵溶液和(B)乙腈的混合溶液作为流动相按程序进行梯度洗脱。质谱测定中采用电喷雾离子源和多反应监测模式。结果表明:22种禁用安神类药物的标准曲线中有17种线性范围为4~800μg·L^-1,有1种为40~8 000μg·L^-1,还有4种为400~80 000μg·L^-1,其检出限(3S/N)为0.02~2μg·g-1。用标准加入法进行回收试验,测得回收率为81.2%~98.9%,测定值的相对标准偏差(n=6)为3.1%~9.7%。展开更多
目的建立高效液相色谱-串联质谱法测定安神类保健品中巴比妥残留的分析方法。方法样品经甲醇-水溶液(50:50, V:V)超声提取、离心、过膜后,经C18色谱柱(50 mm×2.1 mm, 2.6μm)分离,以水和乙腈作为流动相,梯度洗脱。在负电喷雾离子...目的建立高效液相色谱-串联质谱法测定安神类保健品中巴比妥残留的分析方法。方法样品经甲醇-水溶液(50:50, V:V)超声提取、离心、过膜后,经C18色谱柱(50 mm×2.1 mm, 2.6μm)分离,以水和乙腈作为流动相,梯度洗脱。在负电喷雾离子模式下,采用多反应监测模式检测。结果巴比妥在液体和固体基质中的绝对基质效应为4.97%~69.36%,在1.0~50.0 ng/mL范围内线性均良好,相关系数(r^(2))均在0.998以上。巴比妥在0.1、0.5和1.0μg/g3个水平的加标回收率为96.2%~112.0%,相对标准标准偏差为0.10%~6.3%(n=6)。结论本方法操作简单、高效、可靠、灵敏度高,能满足安神类保健品市场的监管和检验需求。展开更多
目的采用替代对照品法建立镇静安神类药物氯氮?、马来酸咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑的高效液相色谱快速检验方法。方法采用Agilent ZORBAX Eclipse Plus C8色谱柱(4.6 mm×150 mm,5μm),流动相:0.01 ...目的采用替代对照品法建立镇静安神类药物氯氮?、马来酸咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑的高效液相色谱快速检验方法。方法采用Agilent ZORBAX Eclipse Plus C8色谱柱(4.6 mm×150 mm,5μm),流动相:0.01 mol·L?1磷酸二氢钾溶液(p H 2.5)-(甲醇-乙腈1∶1)(57∶43),流速:1.0 m L·min?1,柱温:30℃。采用相对容量因子和紫外光谱相似度双指标进行定性;采用相对校正因子法进行定量分析。结果在确定的色谱条件下,氯氮?、咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑完全分离;采用紫外光谱相似度和相对容量因子进行定性,结果准确可靠;采用替代对照品法,计算药物的相对校正因子进行含量测定,能有效减少对照品的使用,加快高效液相色谱分析速度。结论该方法快速、简便、可靠,适用于快速检验镇静安神类药物。展开更多
Objective To report one case of neuroleptic malignant syndrome （NMS） with raising blood sugar. Methods The patient was studied clinically with biochemistry, white blood cells, psychiatric symptoms, and creatine phos...Objective To report one case of neuroleptic malignant syndrome （NMS） with raising blood sugar. Methods The patient was studied clinically with biochemistry, white blood cells, psychiatric symptoms, and creatine phosphokinase （CPK） observations. Results The male patient with a history of taking antipsychot- ics more 30 years and his age of onset was about 20 years. He had severe muscular rigidity, altered consciousness and autonomic disturbance associated with elevation of serum CPK levels （max 3755 U/ L ） and leucocytosis （max 13.3 × 10^9/L）, especially granular leukocytosis（ max 90% ） and lymphocytopenia （rain 8% ）. In addition, high blood sugar emerged along with the variation of white blood cells （ max 9. 0 mmol/L）. Conclusion The manifestations of the patient was in conformity with those of the NMS. The patient had catatonic signs such as mutism, drinking difficulty, etc. and excess of saliva. Developmental observation with CPK and white blood cells is able to reveal the severity level of NMS. Raising blood sugar should be also monitoring item.展开更多
文摘目的采用替代对照品法建立镇静安神类药物氯氮?、马来酸咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑的高效液相色谱快速检验方法。方法采用Agilent ZORBAX Eclipse Plus C8色谱柱(4.6 mm×150 mm,5μm),流动相:0.01 mol·L?1磷酸二氢钾溶液(p H 2.5)-(甲醇-乙腈1∶1)(57∶43),流速:1.0 m L·min?1,柱温:30℃。采用相对容量因子和紫外光谱相似度双指标进行定性;采用相对校正因子法进行定量分析。结果在确定的色谱条件下,氯氮?、咪达唑仑、硝西泮、艾司唑仑、奥沙西泮、劳拉西泮和阿普唑仑完全分离;采用紫外光谱相似度和相对容量因子进行定性,结果准确可靠;采用替代对照品法,计算药物的相对校正因子进行含量测定,能有效减少对照品的使用,加快高效液相色谱分析速度。结论该方法快速、简便、可靠,适用于快速检验镇静安神类药物。
文摘Objective To report one case of neuroleptic malignant syndrome （NMS） with raising blood sugar. Methods The patient was studied clinically with biochemistry, white blood cells, psychiatric symptoms, and creatine phosphokinase （CPK） observations. Results The male patient with a history of taking antipsychot- ics more 30 years and his age of onset was about 20 years. He had severe muscular rigidity, altered consciousness and autonomic disturbance associated with elevation of serum CPK levels （max 3755 U/ L ） and leucocytosis （max 13.3 × 10^9/L）, especially granular leukocytosis（ max 90% ） and lymphocytopenia （rain 8% ）. In addition, high blood sugar emerged along with the variation of white blood cells （ max 9. 0 mmol/L）. Conclusion The manifestations of the patient was in conformity with those of the NMS. The patient had catatonic signs such as mutism, drinking difficulty, etc. and excess of saliva. Developmental observation with CPK and white blood cells is able to reveal the severity level of NMS. Raising blood sugar should be also monitoring item.
