Keywords

Highlights

  • Pharmaceutical analysis in solid samples requires complex extraction method.

  • MeOH:EDTA:McIlvaince buffer is frequently reported as extraction solvent for solids.

  • MeOH:ACN:0.1 M EDTA:McIlvaine extraction buffer is proposed to improve recovery.

  • LC–MS/MS allows multi-residue, sensitive and selective pharmaceuticals analysis.

  • HPLC–UV and HPLC-FLD are still being used due to its lower operating cost.

Introduction

All the while, the trends for analysis of pharmaceuticals in environment are focused in aqueous samples especially on human pharmaceuticals. Unlike human pharmaceuticals, veterinary pharmaceuticals often exist in the complex solid environmental samples such as manure, slurry, and soil. Very few studies have been devoted to pharmaceuticals in solid environmental samples due to pharmaceuticals being a large group of pollutants from different chemical classes with different physico–chemical properties (polar, semi polar, non polar, acidic, basic, neutral, strongly, moderately and weakly sorbed). In this review, we summarized the current available methods for determination of veterinary pharmaceuticals in soil and biological materials; the performance of each method is presented in Table 34.1.

Table 34.1 Methods to determine veterinary pharmaceuticals in different sample matrices
Full size table

Materials and Methods

Sample Preparation and Extraction

Ultrasonic extraction is known as a popular technique which is rapid and does not require large volumes of solvent or expensive instrumentation. This method has been successfully applied to pharmaceuticals extraction in solid environmental samples (Blackwell et al. 2004; Kim and Carlson 2007; Carballo et al. 2007; Aust et al. 2008; Karcı and Balcıoğlu 2009). MeOH: EDTA: McIlvaince buffer was frequently reported as extraction solvent for ultrasonication to extract antibiotics from soil and biosolids (Blackwell et al. 2004; Aust et al. 2008; Karcı and Balcıoğlu 2009). However, this extraction buffer limits to extract only high polarity compounds such as antibiotics whereas low polarity compounds such as hormones are often difficult to extract due to the strong partitioning affinity to soil and organic matter (Ho et al. 2012). Therefore, MeOH:ACN:0.1 M EDTA:McIlvaine buffer was proposed by Ho et al. (2012) to improve the recovery of low polarity analytes.

Instrumental Analysis

Liquid chromatography is widely used as a complementary technique to gas chromatography in residue analysis because of its applicability to the determination of polar, water soluble and non-volatile compounds without derivatization. UV detection (Blackwell et al. 2004; Hu et al. 2008; Karcı and Balcıoğlu 2009), and to a lesser extent mass spectrometry (Haller et al. 2002), and fluorescence detection (Blackwell et al. 2004; Karcı and Balcıoğlu 2009), have been used in the detection techniques in coupled to HPLC, for the analysis of pharmaceuticals in solid environmental samples.

Conclusion

The current available methods for determination of veterinary pharmaceuticals in soil and biological material are reviewed and summarized. In general, most of the extraction methods for veterinary pharmaceuticals in soil and biological materials require ultrasonic extraction with the aid of appropriate extraction buffer and subsequently analyzed by HPLC-FLD or LC–MS/MS.