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Preparation of Biapenem Impurities

Application Introduction

Biapenem is a synthetic antibiotic belonging to carbapenems; its internal is salt-white or off-white powder. During this experiment, two biapenem impurities are separated for structural confirmation.

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Introduction

Biapenem is a synthetic antibiotic belonging to carbapenems; its internal is salt-white or off-white powder. During this experiment, two biapenem impurities are separated for structural confirmation.

Table 1 Biapenem Sample Information

Sample   name

English   name

Structural   formula

Molecular   formula

Molecular   weight

CAS   No.

Biapenem

Biapenem

C215H18N4O4S

350.40

120410-24-4

Experimental

Instrument, reagents and materials

Agela LC-100F high-pressure purification system

Chromatographic solvent: acetonitrile; water: deionized water

HPLC columns: Venusil® XBP C18 (2) (5 µm, 100 Å, 21.2 × 250 mm)

Sample pretreatment

The sample is yellow powder. Add 10 mL of pH3.6 ammonium acetate aqueous solution to 500 mg of the sample, and keep preheating the mixed matter for 1.5 h at 80 °C. Filter the sample with a 0.22 µm membrane, and then perform the sample loading.

Preparation conditions

Chromatographic columns: Venusil® XBP C18 (2) 5 µm, 100 Å, 21.2 × 250 mm;

Mobile phases: A: ammonium acetate aqueous solution (molarity: 0.01 M), B: acetonitrile;

Detector: 220 nm

Flow rate: 12 mL/min

Sample size: 0.6 mL

Gradient:

Table 2 Gradient Elution Conditions of Liquid Chromatography

Time/min

Flow rate/(mL/min)

A/%

B/%

0.0

12.0

95.0

5.0

30.0

12.0

50.0

50.0

Detection conditions

Chromatographic columns: Venusil® XBP C18, 5 µm, 100 Å4.6 × 250 mm;

Mobile phases: Sodium dihydrogen phosphate aqueous solution (molarity: 0.01 M); acetonitrile (proportion: 95:5);

Detector: 220 nm

Flow rate: 1 mL/min

Sample size: 10 µL

Gradient:

Table 3 Gradient Elution Conditions of Liquid Chromatography

Time/min

Flow rate/(mL/min)

A/%

B/%

0.0

1.0

95.0

5.0

30.0

1.0

50.0

50.0

Results and Discussion

In this experiment, biapenem impurities are prepared with Venusil XBP C18 (2) (5 µm, 100 Å, 21.2 × 250 mm) packing. As shown in Table 2 and Figure 1, the sample prepared shows a good peak shape after going through the gradient elution in the mobile phases including ammonium acetate aqueous solution (molarity: 0.01 M) and acetonitrile. Besides, the purity of the product prepared is conforming to the requirement of customer.

Figure 1 Preparation Chromatogram (collection at 8.7 min and distillation at 14.1 min)

Figure 2 Detection Chromatogram of the Product Prepared at 8.7 min

Figure 3 Detection Chromatogram of the Product Prepared at 14.1 min

Conclusion

In this experiment, biapenem impurities are prepared with Venusil® XBP C18 (2) (5 µm, 100 Å, 21.2×250 mm) chromatographic columns. Results show that XBP C18 (2) packing has a good effect on this sample in separation, and the purity of product prepared is conforming to the requirement of customer.

 


  • Venusil XBP C18(2)

    Venusil XBP C18 (2) column's packing material is made with ultra pure silica. The silica surface is processed with Bonna-Agela' s patented surface deactivation technology, followed by a unique bonding process which can reduce the carbon content while maintaining a uniform bonding coverage. The Venusil XBP C18 column does not have excessive retention for highly hydrophobic compounds, and it is great

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