多波长K系数法测定氯芬待因复方片剂的含量

本文报道了多波长Ｋ系数法测定氯芬待因复方片剂中双氯芬酸钠、磷酸可待因两组分含量的研究。结果表明,双氯芬酸钠在１１．１８～２５．４０μｇ／ｍＬ、磷酸可待因在６．７８５～１５．４２μｇ／ｍＬ范围内ΔＡ值与浓度线性关系良好,回归方程分别为ΔＡ双＝－０．００６７４ｃ双－１．４１８５×１０－３,ｒ＝０．９９９６;ΔＡ＝－０．０１３０ｃ可－１．８２２×１０－３,ｒ＝０．９９９８。双氯芬酸钠和磷酸可待因的平均回收率及相对标准偏差分别为１００．１％,０．３６％;１００．７％,０．８０％。方法简便,快速,结果满意。     

多波长线性回归法测定复方氯唑沙宗片中两组分的含量

用多波长线性回归法测定复方氯唑沙宗片中氯唑沙宗对乙酰按基酚的含量。计算程序用ＢＡＳＩＣ语言编制。方法简便、快速,结果满意。     

反相高效液相色谱法测定强力镇痛片中双氯灭痛和阿普唑仑含量

A method fOr simultaneous determination of Liclofenac and Alprazolam in QIANGLI ZHENTONGTablets by RP-HPLC was reported.Chromatographic conditions were:ODS Column as solid phase,Methanol:Water=70:30 as mobile phase, Diclofenac detected at 254nm,Alprazolam detected at 222nm,internal standard:Aminopyrine. The average recoveries of Diclofenac and Alprazolam were 101.37%(n=4)and 102. 73%(n=4)respectively. Coefficients of variation were 1.06%and 1. 73%。 The method was sim-ple,rapid and reliable.     

粉末压片-X-射线荧光光谱法分析砂岩型铀矿制样中粘结剂用量的探讨

由于砂岩型铀矿的成矿特性,样品粉末的内聚力小,采用直接压片法有时难以成型,样片表面常见裂纹,上机测量易碎裂。混合压片法适应性强,制样成功率高,但常见的问题是样品经粘结剂稀释会影响元素的检出限及结果的准确性。本文对粉末压片-X射线荧光光谱法测定砂岩型铀矿地质样品时,前期制样中添加粘结剂的比例进行了研究。试验按照不同比例在铀矿石标准物质GBW04101、GBW04102中添加粘结剂,在扫描电镜下观察到随着粘结剂用量的增加样片表面的光滑度及致密度都呈上升趋势,在X-射线荧光光谱仪上对主量元素进行测定后发现X射线强度在粘结剂添加量大于0.2 g时明显下降,经与GBW04101、GBW04102标准值进行对比后优选出粘结剂与样品的最佳比例为1：20,在此比例下制成的样片光滑平整,不易碎裂,用粉末压片-X射线荧光光谱法进行测定,标准物质测定结果的相对误差为0.56%～6.76 %,相对标准偏差(RSD,n=12)为0.013 %～7.68 %,均达到了《地质矿产实验室测试质量管理规范》DZ/T 0130-2006的要求。本文为粉末压片-X射线荧光光谱法分析砂岩型铀矿地质样品提供了可靠的实验参考依据。     

Comprehensive chemical profiling and quantification of Shexiang Xintongning tablets by integrating liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry

Shexiang Xintongning tablet (SXXTN) is a traditional Chinese medicine (TCM) preparation for the treatment of coronary heart disease (CHD) angina pectoris. However, due to the complexity of the compounds in SXXTN, the active chemical components responsible for the therapeutic effect are still ambiguous. The purpose of our study was to characterize the chemical profile of SXXTN and quantify the representative chemicals. The high-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-QTOF MS) method and gas chromatograph coupled with mass spectrometry (GC–MS) method were utilized to identify the chemical constituents of SXXTN. A total of 140 compounds including alkaloids, ginsenosides, organic acids, esters, triterpenes, phthalides and amino acid were identified in accordance with their retention times, accurate masses and characteristic MS/MS fragment patterns. Forty-four volatile components were characterized by GC–MS through NIST database matching. In the further research of quantitative analysis, 40 non-volatile compounds and 17 volatile compounds were determined and successfully applied for detecting in 7 batches of SXXTN samples by high performance liquid chromatography coupled with triple-quadrupole tandem mass spectrometry (HPLC-QQQ MS) and gas chromatograph coupled with triple-quadrupole tandem mass spectrometry (GC-QQQ MS) in multiple reaction monitoring (MRM) mode, respectively. The quantitative methods were verified in linearity, precision, repeatability stability and recovery. The above results indicated that the established method was practical and reliable for synthetical quality evaluation of SXXTN. In addition, our study might supplement the chemical evidence for disclosing the material basis of its therapeutic effects.