[Study on the proficiency testing program of pharmaceutical preparation analysis].

This proficiency testing program is established to evaluate the pharmaceutical preparation analysis capacity of laboratories recommended by 18 countries and economies. It was authorized by Asia Pacific Laboratory Accreditation Cooperation (APLAC), and organized by Shanghai Institute for Food and Drug Control (SIFDC) and China National Accreditation Service for Conformity Assessment (CNAS). The 0.3sigma test is used to evaluate the homogeneity and stability of the proficiency testing sample. The results of the laboratories were assessed by Z-score. The robust average and the robust standard deviation of the participants' results were calculated as assigned value and standard deviation for performance assessment of hydrochlorothiazide and captopril using robust statistics. Thirty-three of 38 laboratories recommended by 18 countries and economies sent their results back. Twenty-four laboratories' results were observed as satisfactory. Five laboratories were identified as having reported at least one questionable result. Four laboratories were identified as having reported at least one unsatisfactory result.

[Local straight line screening method for the detection of Chinese proprietary medicines containing undeclared prescription drugs].

The present paper constructs a new approach named local straight-line screening (LSLS) to detect Chinese proprietary medicines (CPM) containing undeclared prescription drugs (UPD). Different from traditional methods used in analysis of multi-component spectrum, LSLS is proposed according to the characteristics of original infrared spectra of the UPD and suspected CPM, without any pattern recognition or concentration model establishment. Spectrum-subtraction leads to the variance in local straight line, which serves as a key in discrimination of whether suspected CPD is adulterated or not. Sibutramine hydrochloride, fenfluramine hydrochloride, sildenafil citrate and lovastatin were used as reference substances of UPD to analyze 16 suspected CPM samples. The results show that LSLS can obtain an accurate quantitative and qualitative analysis of suspected CPM. It is possible for the method to be potentially used in the preliminary screening of CPM containing possible UPD.

[Discrimination of adulterated traditional Chinese medicines by infrared spectroscopy-two dimensional correlation analysis].

A new method was established, based on infrared spectroscopy two dimensional (2D) correlation analysis, for the discriminative analysis of adulteration in traditional Chinese medicines (TCM). Fenfluramine hydrochloride (FH) and sibutramine hydrochloride (SH) were taken as examples of synthetic drugs (adulterant), and the correlative peaks of their synchronous 2D correlation spectra were found. Then the characteristics of the synchronous 2D correlation spectrum of the suspected TCM were compared with those of FH. Since the correlative peaks in the synchronous spectrum of the suspected TCM coincide well with those of FH, a positive conclusion could be drawn after further investigation of the asynchronous spectra of TCM, which could provide the information about the source of correlative peaks. On the contrary, the dissimilarity of the synchronous spectra of SH and TCM directly implies that the suspected TCM is not adulterated with SH. The method can be used for a correct discrimination on whether the TCM is adulterated with the synthetic drugs, it does not rely on sample separation, and provides a new simple and cost-effective alternative to test the adulteration of TCM.

The LC-MS/MS methods for the determination of specific antibiotics residues in food matrices.

This chapter describes the LC-MS/MS methods for the determination of antibiotics residues in food matrices. The types of antibiotics include ß-lactam antibiotics, sulfonamides, tetracyclines, fluoroquinolones, nitrofurans, and chloramphenicol (CAP). The food matrices are mainly from animal origin, such as animal tissues, fishes (marine products), eggs, milk, honey, and so on. The methods and procedures are covered, including three parts: (1) Liquid chromatographic conditions, (2) mass spectrometer conditions, including ionization source, analyzer, and acquisition, and (3) extraction and clean-up methods. In each case, the standard operating procedures (SOPs) for analysis are given with sensitivity, linearity, precision, and recovery. Some criteria of maximum residue limits (MRLs) from the legislation are listed.